Water → HCID 21402685, 화합물

HRID 2080108노트

반응식

HRID 2080108 반응식
[C:1]1([S:7][C:8]2[CH:9]=[C:10]([CH:23]=[CH:24][CH:25]=2)[CH2:11][N:12]2C(=O)C3C(=CC=CC=3)C2=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.NN.O>C(O)C>[C:1]1([S:7][C:8]2[CH:9]=[C:10]([CH:23]=[CH:24][CH:25]=2)[CH2:11][NH2:12])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 23130400HCID 23130400, 화합물

생성물 1

HCID 21402685HCID 21402685, 화합물수율 98%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-(3-Phenylsulfanyl-benzyl)-isoindole-1,3-dione described in Preparation Example 94 (123 mg, 0.356 mmol) was dissolved in ethanol (3 mL), hydrazine monohydrate (518 μl, 10.7 mmol) was added at 0° C., and the solution was stirred under reflux for 2 hours. Water was added to the reaction solution at 0° C., which was then extracted with ethyl acetate, the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, the residue was purified by NH silica gel column chromatography (ethyl acetate), and the title compound (75 mg, 0.35 mmol, 98%) was obtained as a colorless oil.

후처리

  1. temperatureunder reflux for 2 hours
  2. extractionwhich was then extracted with ethyl acetate
  3. washthe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated in vacuo
  6. customthe residue was purified by NH silica gel column chromatography (ethyl acetate)

출처 및 근거

ORD 기록
ord-d90ba16cd50348edbcf8767485e31db6
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07932272B2

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