Acrylonitrile → HCID 12926345, 화합물

HRID 893921노트

반응식

HRID 893921 반응식
[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]

참가 물질

4

반응물 2

HCID 7855AcrylonitrileHCID 12926344HCID 12926344, 화합물

생성물 1

HCID 12926345HCID 12926345, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b7dc69c791ca483598404d58348da07e
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04282170

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