Hydrochloric Acid → S-3-(Methylamino)propyl ethanethioate hydrogen chloride salt

HRID 1776675

反応式

HRID 1776675 の反応式
[C:1](=[O:16])([S:3][CH2:4][CH2:5][CH2:6][N:7](C(OC(C)(C)C)=O)[CH3:8])[CH3:2].[ClH:17]>C(O)C.C1(C)C=CC=CC=1>[ClH:17].[C:1](=[O:16])([S:3][CH2:4][CH2:5][CH2:6][NH:7][CH3:8])[CH3:2]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 14194552S-3-(tert-butoxycarbonyl(methyl)amino)propyl ethanethioate

生成物 1

HCID 86644083S-3-(Methylamino)propyl ethanethioate hydrogen chloride salt収率 88%

試薬・触媒・溶媒 1

HCID 21863594Toluene ethanol溶媒

実験手順

S-3-(tert-Butoxycarbonyl(methyl)amino)propyl ethanethioate (206 mg, 0.834 mmol) in 4 ml of EtAc was added 1.0 ml of HCl (conc.) at RT. The mixture was stirred at RT for 1 h, diluted with ethanol/toluene (6 ml, 1:1), evaporated and co-evaporated with ethanol/toluene (3×10 ml), crystallized with ethanol/EtAc/Hexane, filtered, and dried over a vacuum to afford 135 mg (88%) of the title compound. 1H NMR (CDCl3) 9.70 (br, 1H), 8.56 (br, 1H), 3.42 (m, 2H), 2.52 (m, 2H), 2.35 (s, 3H), 2.05 (s, 3H), 1.88 (m, 2H); 13C NMR 174.64, 40.57, 31.57, 27.69, 20.94, 15.62; MS m/z+170.0 (M+Na), 148.10 (M+H).

後処理

  1. customevaporated
  2. customcrystallized with ethanol/EtAc/Hexane
  3. filtrationfiltered
  4. customdried over a vacuum

出典と根拠

ORDレコード
ord-0121f007840144f3bdc1541b5fc4644b
出典データセット
uspto-grants-2016_02
特許番号
US09265841B2

関連ノート

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