Chlorosulfonic acid → HCID 57565301、化合物

HRID 1172182ノート

反応式

HRID 1172182 の反応式
[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]

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 57565267HCID 57565267、化合物

生成物 1

HCID 57565301HCID 57565301、化合物収率 27%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5900e192144d4d2389a6d3c01e117470
出典データセット
uspto-grants-2010_11
特許番号
US07834004B2

反応ノート

読み込み中…