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

HRID 749421ノート

反応式

HRID 749421 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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)+.

後処理

  1. customthe solvent was removed by evaporation

出典と根拠

ORDレコード
ord-160cb4f7171b4b9993e34af73d95aa2b
出典データセット
uspto-grants-2008_07
特許番号
US07402581B2

反応ノート

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