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

HRID 1276175ノート

反応式

HRID 1276175 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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 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.

後処理

  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

出典と根拠

ORDレコード
ord-f05afbec90454e15a93f789a6f12d44d
出典データセット
uspto-grants-2000_12
特許番号
US06166011

反応ノート

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