Benzyl mercaptan → 2-(6-Benzylthiohexyloxy)-5-methyl-1,3-benzenedicarboxaldehyde

HRID 22433

反応式

HRID 22433 の反応式
[O-]CC.[Na+].Br[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[C:18]([CH:19]=[O:20])=[CH:17][C:16]([CH3:21])=[CH:15][C:14]=1[CH:22]=[O:23].[CH2:24]([SH:31])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>C(O)C>[CH2:24]([S:31][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[C:18]([CH:19]=[O:20])=[CH:17][C:16]([CH3:21])=[CH:15][C:14]=1[CH:22]=[O:23])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

参加物

5

反応物 3

HCID 7509Benzyl mercaptanHCID 2723922Sodium ethoxideHCID 199302642-(6-Bromohexyloxy)-5-methyl-1,3-benzenedicarboxaldehyde

生成物 1

HCID 199302892-(6-Benzylthiohexyloxy)-5-methyl-1,3-benzenedicarboxaldehyde

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of sodium ethoxide (69 mg sodium, 3 mmol in ethanol 1 ml) was added to a stirred suspension of 2-(6-bromohexyloxy)-5-methyl-1,3-benzenedicarboxaldehyde (0.98 g, 3 mmol) and benzyl mercaptan (0.35 g, 3 mmol) in ethanol (10 ml) at room temperature under nitrogen. After 1 hour evaporated, water (10 ml) and 2M sodium hydroxide (2 ml) added and extracted with diethyl ether (10 ml). The extracts were washed with water, dried, filtered and evaporated to an oil (1.12 g). Chromatography on silica eluting with dichloromethane gave 2-(6-benzylthiohexyloxy)-5-methyl-1,3-benzenedicarboxaldehyde as a colourless oil.

後処理

  1. customAfter 1 hour evaporated
  2. additionwater (10 ml) and 2M sodium hydroxide (2 ml) added
  3. extractionextracted with diethyl ether (10 ml)
  4. washThe extracts were washed with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated to an oil (1.12 g)

出典と根拠

ORDレコード
ord-7f6483fff6624318bcdbcd4153c44add
出典データセット
uspto-grants-1995_06
特許番号
US05428065

関連ノート

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