Water → 5-Mercapto-4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione

HRID 1730991

反応式

HRID 1730991 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([C:16]2[C:17](=[S:21])[S:18][S:19][CH:20]=2)[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])([CH3:3])[CH3:2].[S-:22][S-].[Na+].[Na+].O>CN(C)C=O>[SH:22][C:20]1[S:19][S:18][C:17](=[S:21])[C:16]=1[C:7]1[CH:6]=[C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[C:10]([OH:11])=[C:9]([C:12]([CH3:14])([CH3:15])[CH3:13])[CH:8]=1

参加物

5

反応物 3

HCID 962WaterHCID 89870Sodium disulfideHCID 98408264-(3,5-Di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione

生成物 1

HCID 214946305-Mercapto-4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

33.8 parts of 4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione and 40 parts of a 2.5 molar solution of sodium disulphide were dissolved in 40 parts of dimethylformamide and warmed at 100°C for 15 minutes. 500 parts of water were then added, the mixture extracted several times with ether to remove any starting material, and then 60 parts of 3N hydrochloric acid solution were added slowly with stirring. The solid was filtered giving 27 parts of 5-mercapto-4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione m.p. 182°C which gave the following elemental analysis:

後処理

  1. extractionthe mixture extracted several times with ether
  2. customto remove any starting material
  3. addition60 parts of 3N hydrochloric acid solution were added slowly
  4. filtrationThe solid was filtered

出典と根拠

ORDレコード
ord-d522f66c7c614c52a078c15ec093d75f
出典データセット
uspto-grants-1976_11
特許番号
US03994923

関連ノート

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