57561-39-4 N-Boc-N-methyl-aminoethanol

Ki te otinga o te 2-(methylamino)ethanol (500 mg, 0.53 ml, 6.66 mmol) i roto i te CH2Cl2 (20 ml) ka taapirihia te Boc2O (1.48 g, 6.79 mmol), ka whai i te whakaoho i te pāmahana rūma mo te 1 haora.I tangohia te otinga tauhohenga ki te tote me te CH2Cl2.I whakamarokehia te paparanga waro ki runga i te MgSO4 ka tātarihia.Na, ko te filtrate i kukū i roto i te korehau ki te tiki i te pūhui ahanoa (hinu taekore, ine);1H NMR (200 MHz, CDCl3) delta 3.74 (q, J= 10.5, 5.2 Hz, 2H) 3.25 (t, J= 5.2 Hz, 2H) 2.91 (s, 3H) 1.45 (s, 9H);tūāwhiorangi papatipu m/e (te kaha whanaunga) 144 (20) 102 (24) 57 (70) 44 (100).
Tauira 38;N1-(3-Fluoro-4-(2-(1-(2-(methylamino)ethyl)-1H-imidazol-4-yl)thieno[3,2-b]pyridin-7-yloxy)phenyl)-N3 -(2-methoxyphenyl)malonamide (96);Hipanga 1: tert-Butyl 2-hydroxyethyl(methyl)carbamate (97) (J. Med. Chem., 1999, 42, 11, 2008) Ki te otinga o te 2-(methylamino)ethanol (5.0 g, 67 mmol) i roto Ko te THF (50 ml) i te RT i taapirihia te Boc2O (15.7 g, 72 mmol) ka whakaohohia te ranunga tauhohenga ki te RT mo nga haora 4.Ko te ranunga tauhohenga i aro ki te maroke, ka whakamahia tika te kohinga taitara 97 i te taahiraa e whai ake nei kaore he purenga atu (11.74 g, 100% te hua).MS (m/z): 176.2 (M+H).
Te Whakaritenga o te l-2-[4-Bromo-2-(4-oxo-2-ftiotaioxo1hiazolidin-5-ylidenemefliyl)phenoxy]efliyl-3-efliyl-l- methylurea(Compoiotamd 161) Hipanga 1 : Te whakahiatotanga o te t-butyl2- hydroxyethylmethylcarbamate;Ki te otinga o te 2-(methylamino)ethanol (500 mg, 0.53 ml, 6.66 mmol) i roto i te CH2Cl2 (20 ml) i tapirihia a BoC2O (1.48 g,6.79 mmol), ka whai i te whakaoho i te pāmahana rūma mo te 1 haora.I tangohia te otinga tauhohenga ki te tote me te CH2Cl2.I whakamarokehia te paparanga waro ki runga i te MgSO4 ka tātarihia.I muri iho, ua haaputuhia te filtrate i roto i te vacuo no te farii i te puohu ahanoa (hinu tae ore, ine);1HNMR (200 MHz, CDCl3) delta 3.74 (q, J= 10.5, 5.2 Hz, 2H) 3.25 (t, J= 5.2 Hz, 2H) 2.91 (s, 3H) 1.45 (s, 9H);tūāwhiorangi papatipu m/e (te kaha whanaunga) 144 (20) 102 (24) 57 (70) 44 (100).
Ko te 2-(methylamino)ethanol (90.1 g, 1.2 mol) i rewa ki te 1.2 L o te methylene chloride, me te BoC2O (218 g, 1 mol) i ata whakaurua ki roto i te whakaohooho i te 00C, ka whai i te pāmahana rūma mo te 3 haora.I horoia te ranunga tauhohenga ki te 700 mL o te wairewa wai o te haukinia haukinia makutu, me te 300 mL wai.I whakamarokehia te ranunga i horoia ma te whakamahi i te konutai konutai konutai, ka kuhu ki raro i te pehanga iti, kia whiwhi ai te pūhui (a) (175 g, 1 mol, 100%) hei hinu kore tae.TLC : Rf = 0.5 (50% EtOAc in Hex) kua whakaatahia me te Ce-Mo stain1H NMR (600MHz, CDCl3) delta 1.47 (s, 9H), 2.88 (br s, IH), 3.41 (br s, 2H), 3.76 (br s, 2H).
90.1 g (1.2 mol) o te 2-(methylamino)ethanol i rewa ki te 1.2 L o te methylene chloride, 218 g (1 mol) o Boc2O i ata tapirihia ki roto i te wa i whakakorikoria ai te otinga i te 0C, ka whakakorikoria te otinga ki te te pāmahana rūma mo te 3 haora.I horoia te ranunga tauhohenga ki te 700 mL o te wairewa haukinia haukinia haukinia me te 300 mL o te wai, ka whakamarokehia ma te whakamahi i te konutai konutai konutai, katahi ka kuhu ki raro i te pehanga iti kia whiwhi 175 g (1 mol) o te puhui hinu achromic e tiakina ana e te Rōpū Boc (hua: 100%).[0140] 1H NMR (600MHz, CDCl3) delta 7.84 (br s, 2H), 7.76 (br s, 2H), 4.34 (d, J = 15.0 Hz, 2H), 3.63 (br s, 2H), 3.04 (d , J = 15.0 Hz, 3H), 1.46 (d, J = 16.2 Hz, 9H) [0141] 90 g (0.514 mol) o te pūhui kua rewa i roto i te 1.5 L o tetrahydrofuran, 88.0 g (539 mol) o N- Ko te hydroxyphthalimide me te 141 g (0.539 mol) o te triphenylphosphine i tapirihia ki roto, 106 mL (0.539 mol) o te diisopropyl azodicarboxylate i ata tapirihia ki runga i te wa e whakakorikoria ana te otinga i te 0C, ka korikori te otinga mo te 3 haora i te whakamahana i te pāmahana. ki te pāmahana rūma.I muri i te kukū o te ranunga tauhohenga i raro i te pehanga iti, ka taapirihia te 600 mL o te isopropylether ki runga, ka whakakorikoria te otinga ki te 0C mo te 1 haora, ka tātarihia te waikura triphenylphosphine momo totoka ma.I horoia te totoka ki te 200 mL o te isopropylether i whakamataohia ki te 0C ka kohia me te filtrate tuatahi, a ko te filtrate ka puta i te kukū i raro i te pehanga iti kia whiwhi 198 g o te ranunga o te Puhui XX me te diisopropyl hydrazodicarboxylate i roto i te tauwehenga whakaranu o te 10 ki te 15% (hua: 120%).[0142] 1H NMR (600MHz, CDCl3) delta 7.84 (br s, 2H), 7.76 (br s, 2H), 4.34 (d, J = 15.0 Hz, 2H), 3.63 (br s, 2H), 3.04 (d , J = 15.0 Hz, 3H), 1.46 (d, J= 16.2 Hz, 9H)