Hydrogen Sulfide → 3-amino-N,N-dimethyl-3-thioxopropanamide

HRID 358477ノート

反応式

HRID 358477 の反応式
[CH3:1][N:2]([CH3:8])[C:3](=[O:7])[CH2:4][C:5]#[N:6].[SH2:9]>C(N(CC)CC)C>[NH2:6][C:5](=[S:9])[CH2:4][C:3]([N:2]([CH3:8])[CH3:1])=[O:7]

参加物

4

反応物 2

HCID 402Hydrogen SulfideHCID 2511432-Cyano-N,N-dimethylacetamide

生成物 1

HCID 27713443-amino-N,N-dimethyl-3-thioxopropanamide

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

反応条件

温度
55 °C

実験手順

A reaction mixture was prepared from 22.4 g. of N,N-dimethylcyanoacetamide, 21 ml. of liquid hydrogen sulfide and 1 ml. of triethylamine. The reaction mixture was placed in an autoclave and the autoclave shaken at about 55° C. for about 12 hours. The reaction mixture was taken from the autoclave and the volatile constituents removed by evaporation. Ethanol was added to the residue, thus producing a crystalline solid. The solid was filtered and the filter cake washed with cold ethanol. Twenty-one grams of 3-amino-3-thioxo-N,N-dimethylpropanamide were obtained melting at 111°-114° C. The compound had the following nmr (CDCl3 +DMSOd6):δ3.07 (doublet, 6H); 3.82 (singlet, 2H); 9.1 (very broad, 1H).

後処理

  1. customA reaction mixture was prepared from 22.4 g
  2. customthe volatile constituents removed by evaporation
  3. additionEthanol was added to the residue
  4. customthus producing a crystalline solid
  5. filtrationThe solid was filtered
  6. washthe filter cake washed with cold ethanol

出典と根拠

ORDレコード
ord-92bbd982283a4134830e172fca60ac6b
出典データセット
uspto-grants-1984_08
特許番号
US04468399

反応ノート

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