Chlorosulfonic acid → 2-Acetyl-7-methoxy-4-benzofuransulphonyl chloride

HRID 979196노트

반응식

HRID 979196 반응식
[C:1]([C:4]1[O:5][C:6]2[C:12]([O:13][CH3:14])=[CH:11][CH:10]=[CH:9][C:7]=2[CH:8]=1)(=[O:3])[CH3:2].[Cl:15][S:16](O)(=[O:18])=[O:17]>>[C:1]([C:4]1[O:5][C:6]2[C:12]([O:13][CH3:14])=[CH:11][CH:10]=[C:9]([S:16]([Cl:15])(=[O:18])=[O:17])[C:7]=2[CH:8]=1)(=[O:3])[CH3:2]

참가 물질

3

반응물 2

HCID 24638Chlorosulfonic acidHCID 39378Ethanone, 1-(7-methoxy-2-benzofuranyl)-

생성물 1

HCID 138514332-Acetyl-7-methoxy-4-benzofuransulphonyl chloride수율 77%

실험 절차

2-Acetyl-7-methoxybenzofuran (5 g) (0.0263 mole) was added to chlorosulfonic acid (18.4 g) (0.158 mole) at -15° C. in portionwise (each 0.5 g) for 30 min. After stirring the reaction mixture at -10° to -5° C. for 1 hour, the resultant was gradually added dropwise to ice. The solution was extracted with ethyl acetate, washed with water and dried, followed by distilling away ethyl acetate under reduced pressure to give 5.8 g of crude 2-acetyl-4-chlorosulfonyl-7-methoxybenzofuran.

후처리

  1. additionthe resultant was gradually added dropwise to ice
  2. extractionThe solution was extracted with ethyl acetate
  3. washwashed with water
  4. customdried
  5. distillationby distilling away ethyl acetate under reduced pressure

출처 및 근거

ORD 기록
ord-60e8caf9630446b79e82c7a4213b37a5
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04666931

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