Chloroacetic Acid → HCID 86739047、化合物

HRID 647131ノート

反応式

HRID 647131 の反応式
[C:1]1([NH:7][C:8]2[S:12][S:11][C:10](=[S:13])[CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:15][C:16]([OH:18])=[O:17].[I-:19].[Na+]>CC(C)=O>[IH:19].[C:1]1([N:7]=[C:8]2[CH:9]=[C:10]([S:13][CH2:15][C:16]([OH:18])=[O:17])[S:11][S:12]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 300Chloroacetic AcidHCID 5238Sodium IodideHCID 13150961HCID 13150961、化合物

生成物 1

HCID 86739047HCID 86739047、化合物収率 43.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
20 °C

実験手順

A solution of 5-phenylamino-1,2-dithiol-3-thione (9 g), chloroacetic acid (4.15 g) and sodium iodide (6.6 g) in acetone (135 cc) is heated under reflux for 35 minutes. After cooling to a temperature of about 20° C., the insoluble product is filtered off and washed successively with acetone (3×15 cc), with water (3×10 cc) and then with acetone (3×10 cc). By recrystallisation of this crude product from methanol (470 cc), (3-phenylimino-1,2-dithiol-5-ylthio)-acetic acid hydroiodide (7.1 g) is obtained, melting at about 205° C. with decomposition.

後処理

  1. temperatureunder reflux for 35 minutes
  2. filtrationthe insoluble product is filtered off
  3. washwashed successively with acetone (3×15 cc), with water (3×10 cc)
  4. customBy recrystallisation of this crude product from methanol (470 cc)

出典と根拠

ORDレコード
ord-d17875c9bd8144369fbf6a9a18276b1c
出典データセット
uspto-grants-1983_10
特許番号
US04407797

反応ノート

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