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Ethyl Acetate → HCID 68821977、化合物

HRID 1817208
ノート
印刷プレビュー

反応式

HRID 1817208 の反応式
[S:1]1(=[O:12])(=[O:11])[C:5]2[CH:6]=[CH:7][C:8]([NH2:10])=[CH:9][C:4]=2[CH2:3][CH2:2]1.[C:13]([C:15](=[CH:21]OCC)[C:16]([O:18][CH2:19][CH3:20])=[O:17])#[N:14].C(OCC)(=O)C>C(O)C>[C:13]([C:15](=[CH:21][NH:10][C:8]1[CH:7]=[CH:6][C:5]2[S:1](=[O:11])(=[O:12])[CH2:2][CH2:3][C:4]=2[CH:9]=1)[C:16]([O:18][CH2:19][CH3:20])=[O:17])#[N:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 789432-Propenoic acid, 2-cyano-3-ethoxy-, ethyl esterHCID 441222602,3-Dihydro-1-benzothiophen-5-amine 1,1-dioxide

生成物 1

HCID 68821977HCID 68821977、化合物収率 82.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5 g (27.3 mmol) of 2,3-dihydro-1-benzothiophen-5-amine 1,1-dioxide were suspended in 50 ml of ethanol under argon, 4.62 g (1 eq, 27.3 mmol) of ethyl 2-cyano-3-ethoxyacrylate were added, and the mixture was heated under reflux overnight. For working up, ethyl acetate was added to the mixture, and the precipitate which formed was filtered off with suction on a frit. The solid was dried in vacuo at 50° C. for 1.5 h. 6.87 g (81%) of the target compound were isolated and were employed without further purification in the next stage.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux overnight
  3. customthe precipitate which formed
  4. filtrationwas filtered off with suction on a frit
  5. customThe solid was dried in vacuo at 50° C. for 1.5 h

出典と根拠

ORDレコード
ord-1df3be3e4d1b425eabb065482162a092
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07598263B2

反応ノート

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