Water → Isobutyric acid 2-acetyl-5-(4-methoxy-benzyloxy)-phenyl ester

HRID 14482

反応式

HRID 14482 の反応式
[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)[CH:5]=[CH:4][C:3]=1[C:18](=[O:20])[CH3:19].C(N(CC)CC)C.[C:28](Cl)(=[O:32])[CH:29]([CH3:31])[CH3:30].O>ClCCl.CN(C)C1C=CN=CC=1>[C:18]([C:3]1[CH:4]=[CH:5][C:6]([O:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)=[CH:7][C:2]=1[O:1][C:28](=[O:32])[CH:29]([CH3:31])[CH3:30])(=[O:20])[CH3:19]

参加物

7

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 62325Isobutyryl chlorideHCID 113232321-(2-Hydroxy-4-((4-methoxyphenyl)methoxy)phenyl)ethanone

生成物 1

HCID 68702579Isobutyric acid 2-acetyl-5-(4-methoxy-benzyloxy)-phenyl ester

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

1-[2-Hydroxy-4-(4-methoxy-benzyloxy)-phenyl]-ethanone (9.11 g, 0.034 mol) is dissolved in dry dichloromethane (120 ml) under an atmosphere of dry argon. Triethylamine (5.14 ml, 0.037 mol) and 4-dimethylaminopyridine (0.204 g, 1.67 mmol) are added, and the mixture is cooled to 0° C. using an ice-water bath. Isobutyryl chloride (3.89 ml, 0.037 mol) is then added dropwise, and the mixture is stirred while warming to room temperature. The mixture is poured into water (100 ml), and the dichloromethane layer is separated, washed with saturated brine (100 ml), dried (MgSO4), treated with activated charcoal (300 mg), filtered and evaporated to give a pale pink solid.

後処理

  1. temperaturewhile warming to room temperature
  2. customthe dichloromethane layer is separated
  3. washwashed with saturated brine (100 ml)
  4. dry with materialdried (MgSO4)
  5. additiontreated with activated charcoal (300 mg)
  6. filtrationfiltered
  7. customevaporated
  8. customto give a pale pink solid

出典と根拠

ORDレコード
ord-f0f1881db2bf48f9b8fc7269f3cdc6c7
出典データセット
uspto-grants-2010_06
特許番号
US07732435B2

関連ノート

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