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Cyclopropylamine → 3-Cyclopropylamino-2-(2,3,4,5-tetrafluorobenzoyl)acrylonitrile

HRID 1788977
ノート
印刷プレビュー

反応式

HRID 1788977 の反応式
[CH:1]1([NH2:4])[CH2:3][CH2:2]1.C(O[CH:8]=[C:9]([C:12](=[O:23])[C:13]1[CH:18]=[C:17]([F:19])[C:16]([F:20])=[C:15]([F:21])[C:14]=1[F:22])[C:10]#[N:11])C>C(Cl)(Cl)Cl.C(O)C.CCCCCC>[CH:1]1([NH:4][CH:8]=[C:9]([C:12](=[O:23])[C:13]2[CH:18]=[C:17]([F:19])[C:16]([F:20])=[C:15]([F:21])[C:14]=2[F:22])[C:10]#[N:11])[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 2

HCID 69828CyclopropylamineHCID 53655523HCID 53655523、化合物

生成物 1

HCID 867417183-Cyclopropylamino-2-(2,3,4,5-tetrafluorobenzoyl)acrylonitrile収率 86.5%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 6212Chloroform溶媒2 回HCID 8058Hexane
溶媒

実験手順

A solution of cyclopropylamine (3.3 g) in chloroform (20 ml) is added dropwise to a solution of 3-ethoxy-2-(2,3,4,5-tetrafluorobenzoyl)acrylonitrile (14.0 g) in chloroform (50 ml) with maintaining the internal temperature between 6° C. and 8° C. by using an ice bath. The mixture is allowed to stand overnight at room temperature and then concentrated under vacuum to yield an orange oily residue. The oily residue is dissolved in ethanol and the ethanol is removed in vacuum to afford a crystalline residue. The residue is dissolved in hexane and washed with a 20:1 mixture of hexane and ethanol to yield 3-cyclopropylamino-2-(2,3,4,5-tetrafluorobenzoyl)acrylonitrile (12.6 g) as pale yellow prisms, m.p. 88°-89° C.

後処理

  1. temperaturewith maintaining the internal temperature between 6° C. and 8° C.
  2. concentrationconcentrated under vacuum
  3. customto yield an orange oily residue
  4. customthe ethanol is removed in vacuum
  5. customto afford a crystalline residue
  6. washwashed with a 20:1 mixture of hexane and ethanol

出典と根拠

ORDレコード
ord-18a86dc2dfb6483390cdb8493d259c89
出典データセット
uspto-grants-1987_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04686221

反応ノート

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