Acetone → N-(1,3-dithiol-2-ylidene)-N-methyl-N-(2-phenyl-1-methoxycarbonylethyl)ammonium iodide

HRID 648905ノート

反応式

HRID 648905 の反応式
CC(C)=O.[CH3:5][O:6][C:7](=[O:18])[C@H:8]([CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[NH:9][CH3:10].[I-:19].CS[C:22]1[S:26][CH:25]=[CH:24][S+:23]=1>O>[I-:19].[S:23]1[CH:24]=[CH:25][S:26][C:22]1=[N+:9]([CH3:10])[CH:8]([C:7]([O:6][CH3:5])=[O:18])[CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 180AcetoneHCID 7021804methyl (2S)-2-(methylamino)-3-phenylpropanoateHCID 19751531(2H-1,3-Dithiol-2-ylidene)(methyl)sulfanium iodide

生成物 1

HCID 14127437N-(1,3-dithiol-2-ylidene)-N-methyl-N-(2-phenyl-1-methoxycarbonylethyl)ammonium iodide収率 55.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 100 ml of acetone, 2.2 g of N-methylphenylalanine methyl ester was dissolved, and 2.0 g of 2-methylthio-1,3-dithiolium iodide was gradually added thereto under stirring at room temperature. The mixture was stirred at room temperature for 1 hour, and then concentrated under reduced pressure. The residue was dissolved in water. The aqueous layer was washed with ethyl acetate, and then water was distilled off under reduced pressure, whereby 1.7 g (yield: 52%) of N-(1,3-dithiol-2-ylidene)-N-methyl-N-(2-phenyl-1-methoxycarbonylethyl)ammonium iodide (Compound No. 5) was obtained as oily substance.

後処理

  1. stirringThe mixture was stirred at room temperature for 1 hour
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe residue was dissolved in water
  4. washThe aqueous layer was washed with ethyl acetate

出典と根拠

ORDレコード
ord-2cbd11fe95fa4042b92d55b8baa71052
出典データセット
uspto-grants-1988_04
特許番号
US04737494

反応ノート

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