Pivaloyl chloride → 1-Benzothiophen-6-YL 2,2-dimethylpropanoate

HRID 732816

반응식

HRID 732816 반응식
[S:1]1[CH:5]=[CH:4][C:3]2[CH:6]=[CH:7][C:8]([OH:10])=[CH:9][C:2]1=2.[CH3:11][C:12]([CH3:17])([CH3:16])[C:13](Cl)=[O:14]>N1C=CC=CC=1>[S:1]1[CH:5]=[CH:4][C:3]2[CH:6]=[CH:7][C:8]([O:10][C:13](=[O:14])[C:12]([CH3:17])([CH3:16])[CH3:11])=[CH:9][C:2]1=2

참가 물질

4

반응물 2

HCID 62493Pivaloyl chlorideHCID 88004Benzo(b)thiophene-6-ol

생성물 1

HCID 690681281-Benzothiophen-6-YL 2,2-dimethylpropanoate수율 98%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Dissolve benzo[b]thiophen-6-ol (10 g, 67 mmol) in pyridine (300 mL). Add 2,2-dimethyl-propionyl chloride (38 mL, 308 mmol) dropwise, and stir at room temperature for 8 hours. Concentrate in vacuo to ¼ volume, partition between ethyl acetate (250 mL) and water (250 mL). Separate layers, wash organic layer with water (250 mL) and brine (200 mL). Dry with magnesium sulfate, filter, and concentrate in vacuo to give 15 g of 2,2-dimethyl-propionic acid benzo[b]thiophen-6-yl ester (98%).

후처리

  1. concentrationConcentrate in vacuo
  2. custompartition between ethyl acetate (250 mL) and water (250 mL)
  3. washSeparate layers, wash organic layer with water (250 mL) and brine (200 mL)
  4. dry with materialDry with magnesium sulfate
  5. filtrationfilter
  6. concentrationconcentrate in vacuo

출처 및 근거

ORD 기록
ord-b9162a7dbdd346cf923519bd1c60a8fd
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585977B2

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