Chlorosulfonic acid → 7-Nitrodibenzo[b,d]furan-2-sulfonyl chloride

HRID 636932ノート

反応式

HRID 636932 の反応式
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[O:9][C:8]=2[CH:16]=1)([O-:3])=[O:2].[Cl:17][S:18](O)(=[O:20])=[O:19]>ClCCl>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[C:11]3[CH:12]=[C:13]([S:18]([Cl:17])(=[O:20])=[O:19])[CH:14]=[CH:15][C:10]=3[O:9][C:8]=2[CH:16]=1)([O-:3])=[O:2]

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 728973-Nitrodibenzofuran

生成物 1

HCID 109030227-Nitrodibenzo[b,d]furan-2-sulfonyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 100 mg of 3-nitrodibenzofuran in 1.7 mL of dichloromethane at −20° C. under a nitrogen atmosphere was added 0.44 mL chlorosulfonic acid in small portions. The reaction mixture was allowed to slowly warm to room temperature and stirred for 66 hours at room temperature. The reaction mixture was poured into ice-cold water, extracted four times with dichloromethane, dried (magnesium sulfate) and concentrated. Purification on silica gel (dichloromethane) yielded 129 mg of 50a: rf=0.73.

後処理

  1. additionThe reaction mixture was poured into ice-cold water
  2. extractionextracted four times with dichloromethane
  3. dry with materialdried (magnesium sulfate)
  4. concentrationconcentrated
  5. customPurification on silica gel (dichloromethane)

出典と根拠

ORDレコード
ord-d668e9cb891f43bd86cb6b09ecb2adbd
出典データセット
uspto-grants-2001_02
特許番号
US06194409B1

反応ノート

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