Propanedioic acid, 1,3-dithiol-2-ylidene-, dimethyl ester → (1,3-Dithiol-2-ylidene)malonic acid monomethyl ester

HRID 129997ノート

反応式

HRID 129997 の反応式
[CH3:1][O:2][C:3](=[O:14])[C:4](=[C:9]1[S:13][CH:12]=[CH:11][S:10]1)[C:5]([O:7]C)=[O:6].[OH-].[K+].CO>CO>[CH3:1][O:2][C:3](=[O:14])[C:4](=[C:9]1[S:13][CH:12]=[CH:11][S:10]1)[C:5]([OH:7])=[O:6]

参加物

4

反応物 2

HCID 9834557Propanedioic acid, 1,3-dithiol-2-ylidene-, dimethyl esterHCID 23689386Potassium hydroxide methanol

生成物 1

HCID 15432125(1,3-Dithiol-2-ylidene)malonic acid monomethyl ester収率 89.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

(1,3-Dithiol-2-ylidene)malonic acid dimethyl ester (232 mg) prepared according to the procedure described in JP-76.48666, was suspended in methanol (0.1 ml) and 1N KOH/methanol (3.0 ml) was added. The reaction mixture was refluxed for 1 h and then concentrated under reduced pressure. The residue was dissolved in water and the pH of the solution was adjusted to 2 with 1N HCl. The resulting precipitate was collected by filtration, washed with water, and dried in vacuo to give the title compound (196 mg) as a pale yellow powder.

後処理

  1. temperatureThe reaction mixture was refluxed for 1 h
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe residue was dissolved in water
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with water
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-cf2d54236d18460183622abfe70fd09b
出典データセット
uspto-grants-1995_11
特許番号
US05470833

反応ノート

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