1-Bromohexane → 5-n-Hexylthio 4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione

HRID 1730992

反応式

HRID 1730992 の反応式
[Na].[SH:2][C:3]1[S:7][S:6][C:5](=[S:8])[C:4]=1[C:9]1[CH:14]=[C:13]([C:15]([CH3:18])([CH3:17])[CH3:16])[C:12]([OH:19])=[C:11]([C:20]([CH3:23])([CH3:22])[CH3:21])[CH:10]=1.[CH2:24](Br)[CH2:25][CH2:26][CH2:27][CH2:28][CH3:29]>C(O)C>[CH2:24]([S:2][C:3]1[S:7][S:6][C:5](=[S:8])[C:4]=1[C:9]1[CH:14]=[C:13]([C:15]([CH3:16])([CH3:17])[CH3:18])[C:12]([OH:19])=[C:11]([C:20]([CH3:23])([CH3:22])[CH3:21])[CH:10]=1)[CH2:25][CH2:26][CH2:27][CH2:28][CH3:29]

参加物

5

反応物 3

HCID 81011-BromohexaneHCID 5360545SodiumHCID 214946305-Mercapto-4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione

生成物 1

HCID 98685945-n-Hexylthio 4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒3 回

反応条件

温度
50 °C

実験手順

0.92 parts of sodium was dissolved in 80 parts of ethanol and to this was added 14.8 parts of 5-mercapto-4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione, as prepared in example 11 dissolved in 200 parts ethanol. The mixture was then warmed to 50°C and a solution of 6.6 parts n-hexyl bromide in 50 parts ethanol was added dropwise. The mixture was refluxed for 5 hours, the ethanol evaporated, and the residue extracted with diethyl ether. Evaporation of the ether solution gave a crystalline residue which was crystallised from ether to give 12 parts of 5-n-hexylthio 4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione, m.p. 110°.

後処理

  1. customas prepared in example 11
  2. temperatureThe mixture was refluxed for 5 hours
  3. customthe ethanol evaporated
  4. extractionthe residue extracted with diethyl ether
  5. customEvaporation of the ether solution
  6. customgave a crystalline residue which
  7. customwas crystallised from ether

出典と根拠

ORDレコード
ord-0255547498fd49348e78a655574d2eca
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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