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Water → C-(5-(2-Cyclopropylvinyl)thiophen-2-yl)methylamine

HRID 2080141
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HRID 2080141 반응식
[CH:1]1([CH:4]=[CH:5][C:6]2[S:10][C:9]([CH2:11][N:12]3C(=O)C4C(=CC=CC=4)C3=O)=[CH:8][CH:7]=2)[CH2:3][CH2:2]1.O.NN.[OH-].[Na+].O>C(O)C>[CH:1]1([CH:4]=[CH:5][C:6]2[S:10][C:9]([CH2:11][NH2:12])=[CH:8][CH:7]=2)[CH2:3][CH2:2]1
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참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 671195832-(5-(2-Cyclopropylvinyl)thiophen-2-ylmethyl)isoindol-1,3-dione

생성물 1

HCID 67119557C-(5-(2-Cyclopropylvinyl)thiophen-2-yl)methylamine수율 98.6%

시약·촉매·용매 1

HCID 702
Ethanol
용매

실험 절차

2-(5-(2-Cyclopropylvinyl)thiophen-2-ylmethyl)isoindol-1,3-dione described in Preparation Example 150 (330 mg, 1.02 mmol) was dissolved in ethanol (50 mL), hydrazine monohydrate (500 mg, 10 mmol) was added thereto, and the solution was stirred under reflux for 2 hours. After cooling to room temperature, 2N sodium hydroxide solution (10 mL) and water (100 mL) were added to the reaction solution, which was then washed twice with hexane (50 mL). The organic layer was dried over anhydrous sodium sulfate, then, the solvent was evaporated in vacuo, and the title compound (180 mg, 1.01 mmol, 98.6%) was obtained as a colorless oil.

후처리

  1. temperatureunder reflux for 2 hours
  2. washwas then washed twice with hexane (50 mL)
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated in vacuo

출처 및 근거

ORD 기록
ord-527b9a0adfba491888f8de2e74143a9a
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932272B2

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