Acrylonitrile → HCID 12926345、化合物

HRID 893921ノート

反応式

HRID 893921 の反応式
[CH3:1][NH:2][C:3]([CH:5]1[C:17]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[C:11]2[C:6]1=[CH:7][CH:8]=[CH:9][CH:10]=2)=[O:4].[C:18](#[N:21])[CH:19]=[CH2:20]>O1CCCC1>[C:18]([CH2:19][CH2:20][C:5]1([C:3](=[O:4])[NH:2][CH3:1])[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=2[C:12]2[C:17]1=[CH:16][CH:15]=[CH:14][CH:13]=2)#[N:21]

参加物

4

反応物 2

HCID 7855AcrylonitrileHCID 12926344HCID 12926344、化合物

生成物 1

HCID 12926345HCID 12926345、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A 36.8 g. portion of 9-(N-methylcarbamoyl)fluorene was reacted with 10.6 g. of acrylonitrile in the presence of 10 g. of Triton B in tetrahydrofuran as described in Example 4. The reaction mixture was then concentrated under vacuum to a semi-solid, which was added to ice-water/ethyl acetate. The organic layer was separated, washed with water, and dried over sodium sulfate. The solution was evaporated to dryness to obtain 45.8 g. of crude product, which was crystallized from ethyl acetate/hexane to obtain 30 g. of the desired product, m.p. 185°-187°. Infrared analysis of the product showed a carbonyl band at 1685 cm-1 and a nitrile band at 2270 cm-1.

後処理

  1. concentrationThe reaction mixture was then concentrated under vacuum to a semi-solid, which
  2. additionwas added to ice-water/ethyl acetate
  3. customThe organic layer was separated
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. customThe solution was evaporated to dryness
  7. customto obtain 45.8 g
  8. customof crude product, which was crystallized from ethyl acetate/hexane
  9. customto obtain 30 g

出典と根拠

ORDレコード
ord-b7dc69c791ca483598404d58348da07e
出典データセット
uspto-grants-1981_08
特許番号
US04282170

反応ノート

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