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

HRID 1730991

반응식

HRID 1730991 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-d522f66c7c614c52a078c15ec093d75f
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03994923

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