Hydrochloric Acid → 2-Methylbutyl 4-dimethylsilylbenzoate

HRID 1197728

反応式

HRID 1197728 の反応式
[CH3:1][SiH:2]([CH3:12])[C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][CH:4]=1.[CH3:13][CH:14]([CH2:17][CH3:18])[CH2:15][OH:16].Cl>N1C=CC=CC=1>[CH3:1][SiH:2]([CH3:12])[C:3]1[CH:11]=[CH:10][C:6]([C:7]([O:16][CH2:15][CH:14]([CH3:13])[CH2:17][CH3:18])=[O:8])=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 87232-Methyl-1-butanolHCID 71434831p-Dimethylsilylbenzoyl chloride

生成物 1

HCID 1235240052-Methylbutyl 4-dimethylsilylbenzoate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
25 °C

実験手順

20.0 g (0.101 mol) of 4-dimethylsilylbenzoyl chloride were added dropwise at 10° C.-15° C. to a solution of 8.90 g (0.101 mol) of 2-methylbutan-1-ol in 20 ml of dry pyridine. The reaction solution was stirred for one hour at 25° C., poured onto ice and acidified using HCl. The organic phase was separated off, diluted with toluene and washed by shaking three times with 10% HCl. It was washed with water and dried over sodium sulfate. After the toluene had been stripped off in vacuo on a rotary evaporator, distillation gave 2-methylbutyl 4-dimethylsilylbenzoate; boiling point 86° C.-110° C./0.05 mmHg.

後処理

  1. additionpoured onto ice
  2. customThe organic phase was separated off
  3. additiondiluted with toluene
  4. washwashed
  5. stirringby shaking three times with 10% HCl
  6. washIt was washed with water
  7. dry with materialdried over sodium sulfate
  8. customAfter the toluene had been stripped off in vacuo on a rotary evaporator, distillation

出典と根拠

ORDレコード
ord-6ffafd9ff23542d2a3db6da01bd2f2d4
出典データセット
uspto-grants-1994_01
特許番号
US05277838

関連ノート

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