Sodium hydride → 3-(2-Benzyl-4-chlorophenyl)prop-2-enenitrile

HRID 1462635ノート

反応式

HRID 1462635 の反応式
[H-].[Na+].P(=O)([O-])O[C:5](CC)(CC)[C:6]#[N:7].[CH2:14]([C:21]1[CH:28]=[C:27]([Cl:29])[CH:26]=[CH:25][C:22]=1[CH:23]=O)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>O1CCCC1>[CH2:14]([C:21]1[CH:28]=[C:27]([Cl:29])[CH:26]=[CH:25][C:22]=1[CH:23]=[CH:5][C:6]#[N:7])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 155700672-Benzyl-4-chlorobenzaldehydeHCID 178449162HCID 178449162、化合物

生成物 1

HCID 545603803-(2-Benzyl-4-chlorophenyl)prop-2-enenitrile

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of 10.5 g (0.437 mole) of mineral oil free sodium hydride in 1.2 liters of tetrahydrofuran was added dropwise 58.4 g (0.328 mole) of diethylcyanomethyl phosphonate. After the hyrogen evolution had ceased ca 60 min, 69.4 g (0.3 mole) of 2-benzyl-4-chlorobenzaldehyde, in 75 ml of tetrahydrofuran was added dropwise. The mixture was stirred overnight at room temperature. The tetrahydrofuran solution was decanted, and concentrated at room temperature. The residue was partitioned between 2 liters of water and 1.5 liters of ether. The ether solution was separated, washed with water, and dried with sodium sulfate. The ether was removed at reduced pressure to give a yellow oil which was used without further purification.

後処理

  1. waitAfter the hyrogen evolution had ceased ca 60 min
  2. customThe tetrahydrofuran solution was decanted
  3. concentrationconcentrated at room temperature
  4. customThe residue was partitioned between 2 liters of water and 1.5 liters of ether
  5. customThe ether solution was separated
  6. washwashed with water
  7. dry with materialdried with sodium sulfate
  8. customThe ether was removed at reduced pressure
  9. customto give a yellow oil which
  10. customwas used without further purification

出典と根拠

ORDレコード
ord-b484407e529d4e60912c8b315b9cf3c7
出典データセット
uspto-grants-1984_07
特許番号
US04460781

反応ノート

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