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Ethyl 2-azido-3-(5-methylthiophen-2-yl)acrylate → ethyl 2-methyl-4H-thieno[3,2-b]pyrrole-5-carboxylate

HRID 518124
ノート
印刷プレビュー

反応式

HRID 518124 の反応式
[N:1]([C:4](=[CH:10][C:11]1[S:12][C:13]([CH3:16])=[CH:14][CH:15]=1)[C:5]([O:7][CH2:8][CH3:9])=[O:6])=[N+]=[N-]>C1(C)C=CC=C(C)C=1>[CH3:16][C:13]1[S:12][C:11]2[CH:10]=[C:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[NH:1][C:15]=2[CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 76601917Ethyl 2-azido-3-(5-methylthiophen-2-yl)acrylate

生成物 1

HCID 1438928ethyl 2-methyl-4H-thieno[3,2-b]pyrrole-5-carboxylate収率 85.9%

試薬・触媒・溶媒 1

HCID 7929M-Xylene溶媒

実験手順

Ethyl 2-azido-3-(5-methylthiophen-2-yl)acrylate (3.38 g) was dissolved in m-xylene (30 mL) and the mixture was heated at reflux for 1 hour. The reaction solution was concentrated under reduced pressure. To the residue was added n-hexane and the residue was washed with n-hexane. The solid was collected by filtration, and dried under reduced pressure to give the title compound (2.56 g).

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 1 hour
  3. concentrationThe reaction solution was concentrated under reduced pressure
  4. additionTo the residue was added n-hexane
  5. washthe residue was washed with n-hexane
  6. filtrationThe solid was collected by filtration
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-98005136887b4bbd8f6d888542a7406e
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09115144B2

反応ノート

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