Acetic Anhydride → 2-Chloro-1,3-benzoxazol-6-yl acetate

HRID 1635658노트

반응식

HRID 1635658 반응식
C(N(CC)CC)C.[Cl:8][C:9]1[O:10][C:11]2[CH:17]=[C:16]([OH:18])[CH:15]=[CH:14][C:12]=2[N:13]=1.[C:19](OC(=O)C)(=[O:21])[CH3:20]>ClCCl>[C:19]([O:18][C:16]1[CH:15]=[CH:14][C:12]2[N:13]=[C:9]([Cl:8])[O:10][C:11]=2[CH:17]=1)(=[O:21])[CH3:20]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 234412462-Chloro-1,3-benzoxazol-6-OL

생성물 1

HCID 183401792-Chloro-1,3-benzoxazol-6-yl acetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Triethylamine (1.48 ml) was added to a suspension of 2-chloro-1,3-benzoxazol-6-ol (1.63 g) [see Preparation 34] in dichloromethane (20 ml), and after 5 minutes acetic anhydride (1.01 ml) was added. The reaction mixture was stirred at room temperature for 18 hours, after which time the solvent was removed under reduced pressure. The crude product was purified by column chromatography on silica gel eluting with a solvent gradient of 100:0, changing to 40:10, changing to 0:100, by volume, hexane:ethyl acetate to afford 2-chloro-1,3-benzoxazol-6-yl acetate (1.63 g) as an oil.

후처리

  1. customafter which time the solvent was removed under reduced pressure
  2. customThe crude product was purified by column chromatography on silica gel eluting with a solvent gradient of 100:0

출처 및 근거

ORD 기록
ord-6437e919629846eabefddf4632cf1e9e
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06509464B1

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