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

HRID 979196ノート

反応式

HRID 979196 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

HCID 138514332-Acetyl-7-methoxy-4-benzofuransulphonyl chloride収率 77%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-60e8caf9630446b79e82c7a4213b37a5
出典データセット
uspto-grants-1987_05
特許番号
US04666931

反応ノート

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