Water → Indapamide

HRID 1589422노트

반응식

HRID 1589422 반응식
[CH2:1]([N:4]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[NH:5][C:6](=O)[C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[C:9]([S:14](=[O:17])(=[O:16])[NH2:15])[CH:8]=1)[CH:2]=[CH2:3].[OH2:25]>Cl.Cl.[Cl-].[Cl-].[Zn+2].[Cl-].[Zn+2].[Cl-]>[Cl:13][C:10]1[CH:11]=[CH:12][C:7]([C:6]([NH:5][N:4]2[C:1]3[C:21](=[CH:22][CH:23]=[CH:3][CH:2]=3)[CH2:20][CH:19]2[CH3:24])=[O:25])=[CH:8][C:9]=1[S:14](=[O:16])(=[O:17])[NH2:15]

참가 물질

6

반응물 2

HCID 962WaterHCID 155715021-Allyl-1-phenyl-2-(3-sulfamoyl-4-chlorobenzoyl)-hydrazine

생성물 1

HCID 3702Indapamide

시약·촉매·용매 3

HCID 3007855Zincchloride촉매HCID 21263579ZINC chloride hydrogen chloride촉매HCID 313Hydrochloric Acid용매

실험 절차

In a 50 ml round bottom was placed 8 grams of Lucas reagent. The reagent is prepared by dissolving 16 grams of anhydrous zinc chloride in 10 ml of concentrated hydrochloric acid. To this reagent was added 100 mg (0.27 mmols) of 1-allyl-1-phenyl-2-(3-sulfamoyl-4-chlorobenzoyl)-hydrazine with stirring under nitrogen for a short time to dissolve the solid. The reaction cyclized at 60° C. over 6 hours. The reactant was worked up by pouring the cooled reaction mixture into water and extracting the product into ethyl acetate. The ethyl acetate phase was cross washed several times with water and sodium bicarbonate solution. The ethyl acetate solution is dried with magnesium sulfate, clarified and evaporated to dryness yielding 84 mg of crude 1-(4-chloro-3-sulfamoylbenzamido)-2-methylindoline.

후처리

  1. customThe reagent is prepared
  2. dissolutionto dissolve the solid
  3. additionby pouring
  4. extractionextracting the product into ethyl acetate
  5. dry with materialThe ethyl acetate solution is dried with magnesium sulfate
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-e8e0c6a26c7f43feac79a0a4b0e6e1cb
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04570001

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