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

HRID 14482

반응식

HRID 14482 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f0f1881db2bf48f9b8fc7269f3cdc6c7
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732435B2

연결된 노트

불러오는 중…