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

HRID 461868

反応式

HRID 461868 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 544628003-Tert-butyl-4-hydroxy-5-iodobenzylidenemalononitrile収率 84.3%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 962Water溶媒

実験手順

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°.

後処理

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

出典と根拠

ORDレコード
ord-6264988a23e04841afde046a04b55b72
出典データセット
uspto-grants-1977_12
特許番号
US04064266

関連ノート

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