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p-Toluenesulfonic acid → HCID 54501125, 화합물

HRID 904823
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HRID 904823 반응식
[CH:1]([S:4]([N:7]1[C:11]2[CH:12]=[C:13]([C:16](O)([CH2:23][C:24]([O:26][CH3:27])=[O:25])[C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[NH2:29])(=[O:6])=[O:5])([CH3:3])[CH3:2].C1(C)C=CC(S(O)(=O)=O)=CC=1>C(Cl)(Cl)Cl>[CH:1]([S:4]([N:7]1[C:11]2[CH:12]=[C:13]([C:16](=[CH:23][C:24]([O:26][CH3:27])=[O:25])[C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[NH2:29])(=[O:5])=[O:6])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6101p-Toluenesulfonic acidHCID 132864971-Isopropylsulfonyl-2-amino-6-(alpha-hydroxy-alpha-methoxycarbonylmethylbenzyl)benzimidazole

생성물 1

HCID 54501125HCID 54501125, 화합물수율 96%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A solution of 6.0 g. of 1-isopropylsulfonyl-2-amino-6-(α-hydroxy-α-methoxycarbonylmethylbenzyl)benzimidazole (from Example 4) and 6.0 g. of p-toluenesulfonic acid in 150 ml. of chloroform was heated at reflux for three hours. The solution was cooled to room temperature and washed two times with saturated aqueous sodium bicarbonate solution, and two times with water. After drying the solution over sodium sulfate, the solvent was removed by evaporation under reduced pressure to provide 5.5 g. (96% yield) of 1-isopropylsulfonyl-2-amino-6-(α-methoxycarbonylmethylenebenzyl)benzimidazole. M.P. 160°-165° C.

후처리

  1. temperatureat reflux for three hours
  2. washwashed two times with saturated aqueous sodium bicarbonate solution, and two times with water
  3. dry with materialAfter drying the solution over sodium sulfate
  4. customthe solvent was removed by evaporation under reduced pressure
  5. customto provide 5.5 g

출처 및 근거

ORD 기록
ord-9bd714e4559943ccaab3c2ad4ebc3d47
출처 데이터셋
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04420479

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