Water → 2-Thioxo-[1,3]dithiole-4-carboxylic acid methyl ester

HRID 1682092ノート

反応式

HRID 1682092 の反応式
[S:1]1[C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4](C(OC)=O)[S:3][C:2]1=[S:14].O.[Br-].[Li+].O>CN(C)P(=O)(N(C)C)N(C)C>[S:3]1[CH:4]=[C:5]([C:6]([O:8][CH3:9])=[O:7])[S:1][C:2]1=[S:14]

参加物

5

反応物 3

HCID 962WaterHCID 547914Dimethyl 2-thioxo-1,3-dithiole-4,5-dicarboxylateHCID 23702478Lithium bromide hydrate

生成物 1

HCID 108671782-Thioxo-[1,3]dithiole-4-carboxylic acid methyl ester収率 70%

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide溶媒

実験手順

30 Grams (0.12 mol) of dimethyl 1,3-dithiol-2-thion-4,5-dicarboxylate synthesized according to the method of G. C. Papavassiliou, et al [Synthetic Metals, Vol. 27 (1988) B-373-B378] was dissolved in 30 ml of hexamethylphosphorictriamide (HMPA), and 12.6 g (0.12 mol) of lithium bromide monohydrate was added. The resultant mixture was heated at 60° C. for 1 hour, the reaction mixture was allowed to cool to room temperature, 200 ml of water was added, and a yellow solid formed was separated by filtering and washed with water. The solid obtained was dried and recrystallized from carbon tetrachloride to give 16.2 g of yellow acicular crystals of methyl 1,3-dithiol-2-thione-4-carboxylate (yield 70%).

後処理

  1. customa yellow solid formed
  2. customwas separated
  3. filtrationby filtering
  4. washwashed with water
  5. customThe solid obtained
  6. customwas dried
  7. customrecrystallized from carbon tetrachloride

出典と根拠

ORDレコード
ord-f386a8c6f8bd459a858c1a15a2649769
出典データセット
uspto-grants-1992_12
特許番号
US05175280

反応ノート

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