Hydrochloric Acid → [(2S)-2-(3,4-dichlorophenyl)-4-(3-thiomorpholin-4-ylazetidin-1-yl)butyl]methylamine dihydrochloride

HRID 749421노트

반응식

HRID 749421 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C@H:9]([CH2:20][CH2:21][N:22]2[CH2:25][CH:24]([N:26]3[CH2:31][CH2:30][S:29][CH2:28][CH2:27]3)[CH2:23]2)[CH2:10][N:11](C)[C:12](=O)OC(C)(C)C)[CH:5]=[CH:6][C:7]=1[Cl:8].[ClH:32]>CCOCC>[ClH:1].[ClH:32].[Cl:1][C:2]1[CH:3]=[C:4]([C@H:9]([CH2:20][CH2:21][N:22]2[CH2:23][CH:24]([N:26]3[CH2:27][CH2:28][S:29][CH2:30][CH2:31]3)[CH2:25]2)[CH2:10][NH:11][CH3:12])[CH:5]=[CH:6][C:7]=1[Cl:8]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86606876tert-butyl [(2S)-2-(3,4-dichlorophenyl)-4-(3-thiomorpholin-4-ylazetidin-1-yl)butyl]methylcarbamate

생성물 1

HCID 68979570[(2S)-2-(3,4-dichlorophenyl)-4-(3-thiomorpholin-4-ylazetidin-1-yl)butyl]methylamine dihydrochloride수율 100%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

tert-Butyl [(2S)-2-(3,4-dichlorophenyl)-4-(3-thiomorpholin-4-ylazetidin-1-yl)butyl]methylcarbamate (260 mg, 0.53 mmol) was dissolved in ether (15 mL) and stirred during the dropwise addition of HCl (15 mL of 4M dioxane solution). The mixture was stirred at room temperature for 1 h and then the solvent was removed by evaporation. There was obtained 270 mg (100%) of [(2S)-2-(3,4-dichlorophenyl)-4-(3-thiomorpholin-4-ylazetidin-1-yl)butyl]methylamine dihydrochloride as a white solid. 1H NMR (300 MHz, CD3OD): 1.9-2.2 (b, 2H), 2.7 (s, 3H), 3.0-4.8 (cm, 19H), 7.4 (d, 1H), 7.6 (m, 2H); LCMS: m/z 388 (M+1)+.

후처리

  1. customthe solvent was removed by evaporation

출처 및 근거

ORD 기록
ord-160cb4f7171b4b9993e34af73d95aa2b
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07402581B2

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