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

HRID 2080141
ノート
印刷プレビュー

反応式

HRID 2080141 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-527b9a0adfba491888f8de2e74143a9a
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932272B2

反応ノート

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