Acetic Acid → 3-Tert-butyl-4-hydroxy-5-iodobenzylidenemalononitrile

HRID 461868

반응식

HRID 461868 반응식
[C:1]([C:5]1[CH:6]=[C:7]([CH:10]=[C:11]([I:14])[C:12]=1[OH:13])[CH:8]=O)([CH3:4])([CH3:3])[CH3:2].[C:15](#[N:19])[CH2:16][C:17]#[N:18].N1CCCCC1.C(O)(=O)C>O.C1C=CC=CC=1>[C:1]([C:5]1[CH:6]=[C:7]([CH:10]=[C:11]([I:14])[C:12]=1[OH:13])[CH:8]=[C:16]([C:15]#[N:19])[C:17]#[N:18])([CH3:4])([CH3:3])[CH3:2]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 8010MalononitrileHCID 8082PiperidineHCID 186773843-Tert-butyl-4-hydroxy-5-iodobenzaldehyde

생성물 1

HCID 544628003-Tert-butyl-4-hydroxy-5-iodobenzylidenemalononitrile수율 84.3%

시약·촉매·용매 2

HCID 241Benzene용매HCID 962Water용매

실험 절차

3-tert-butyl-4-hydroxy-5-iodobenzaldehyde (24.8 gm), malononitrile (6.2 gm), piperidine (1.0 ml), acetic acid (3.3 ml) and benzene (300 ml) were refluxed under a Dean and Stark water separator for 2 hours. On cooling a crystalline precipitate formed and was filtered off. Recrystallisation from ethylene dichloride gave pale yellow needles of 3-tert-butyl-4-hydroxy-5-iodobenzylidenemalononitrile (24.2 gm) m.p. 188°.

후처리

  1. temperatureOn cooling a crystalline precipitate
  2. customformed
  3. filtrationwas filtered off
  4. customRecrystallisation from ethylene dichloride

출처 및 근거

ORD 기록
ord-6264988a23e04841afde046a04b55b72
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04064266

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