Chlorosulfonic acid → HCID 57565301, 화합물

HRID 1727061노트

반응식

HRID 1727061 반응식
[N+:1]([C:4]1[CH:22]=[CH:21][C:7]([CH2:8][O:9][C:10]([CH:12]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[CH2:14][CH2:13]2)=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].[Cl:23][S:24](O)(=[O:26])=[O:25]>C(Cl)(Cl)Cl>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([CH2:8][O:9][C:10]([CH:12]2[C:20]3[C:15](=[CH:16][CH:17]=[C:18]([S:24]([Cl:23])(=[O:26])=[O:25])[CH:19]=3)[CH2:14][CH2:13]2)=[O:11])=[CH:21][CH:22]=1)([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 57565267HCID 57565267, 화합물

생성물 1

HCID 57565301HCID 57565301, 화합물수율 27%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of indan-1-carboxylic acid 4-nitro-benzyl ester (2.3 g, 8.1 mmol) in anhydrous CHCl3 (13 mL) at −20° C. was added chlorosulfonic acid (2.8 g, 24.0 mmol) over a period of 10 minutes. The mixture was warmed to ambient temperature and stirred for 16 h. The reaction mixture was combined with ice-water and the resulting layer was extracted with CH2Cl2. The CH2Cl2 layer was washed with brine and was dried over anhydrous Na2SO4. The crude product was purified using flash silica chromatography (0-30% EtOAc/Hex) to yield 0.84 g (27%) of 6-chlorosulfonyl-indan-1-carboxylic acid 4-nitro-benzyl ester.

후처리

  1. extractionthe resulting layer was extracted with CH2Cl2
  2. washThe CH2Cl2 layer was washed with brine
  3. dry with materialwas dried over anhydrous Na2SO4
  4. customThe crude product was purified

출처 및 근거

ORD 기록
ord-eb67d2288f0c4c7096f568c2d0b0aa78
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07494999B2

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