Water → HCID 14820516, 화합물

HRID 1088830노트

반응식

HRID 1088830 반응식
[NH2:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[CH2:7][CH:6]([NH:11][S:12]([C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=1)(=[O:14])=[O:13])[CH2:5]2.C(=O)([O-])O.[Na+].Br[CH2:28][C:29]([O:31][CH3:32])=[O:30].O>CN(C)P(=O)(N(C)C)N(C)C>[Cl:21][C:18]1[CH:19]=[CH:20][C:15]([S:12]([NH:11][CH:6]2[CH2:5][C:4]3[C:8](=[CH:9][CH:10]=[C:2]([NH:1][CH2:28][C:29]([O:31][CH3:32])=[O:30])[CH:3]=3)[CH2:7]2)(=[O:14])=[O:13])=[CH:16][CH:17]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 60984Methyl bromoacetateHCID 516892Sodium BicarbonateHCID 14820515HCID 14820515, 화합물

생성물 1

HCID 14820516HCID 14820516, 화합물수율 77%

시약·촉매·용매 1

HCID 12679Hexamethylphosphoramide용매

실험 절차

Into a solution of 0.5 g of 5-amino-2-(4-chlorophenyl)sulfonylaminoindan in 5 ml of hexamethylphosphoric triamide are added 0.2 g of sodium hydrogen carbonate and 0.25 g of methyl bromoacetate at 5 to 10° C., and the mixture is stirred at the same temperature for 4 hours. Water is added to the reaction mixture, followed by extraction with ethyl acetate. The extract is washed, dried and the solvent is evaporated. The residue is purified by separation through silica gel column chromatography (eluant: chloroform : ethyl acetate=7 : 3), and further recrystallized from ethyl acetate-n-hexane mixture to give 0.47 g of methyl N-[2-(4-chlorophenyl)sulfonylaminoindan-5-yl]glycinate.

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe extract is washed
  3. customdried
  4. customthe solvent is evaporated
  5. customThe residue is purified by separation through silica gel column chromatography (eluant: chloroform : ethyl acetate=7 : 3)
  6. customfurther recrystallized from ethyl acetate-n-hexane mixture

출처 및 근거

ORD 기록
ord-1527583dc1524b90a427baeccfd6e80e
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04963587

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