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

HRID 1279029노트

반응식

HRID 1279029 반응식
[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]

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 728973-Nitrodibenzofuran

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-6cb589b2537646cc9651ffdbb80e9e08
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06444672B1

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