Sodium → HCID 178444383、化合物

HRID 1463013ノート

反応式

HRID 1463013 の反応式
C(O[CH:4]=[C:5]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][CH2:16][CH3:17])=[CH:10][CH:9]=1)[CH:6]=O)C.Cl.[CH2:19]([C@H:24]1[CH2:29][CH2:28][C@H:27]([C:30]([NH2:32])=[NH:31])[CH2:26][CH2:25]1)[CH2:20][CH2:21][CH2:22][CH3:23].C[O-].[Na+].[Na]>CO>[CH2:19]([C@H:24]1[CH2:25][CH2:26][C@H:27]([C:30]2[N:31]=[CH:4][C:5]([C:8]3[CH:9]=[CH:10][C:11]([CH2:14][CH2:15][CH2:16][CH3:17])=[CH:12][CH:13]=3)=[CH:6][N:32]=2)[CH2:28][CH2:29]1)[CH2:20][CH2:21][CH2:22][CH3:23]

参加物

6

反応物 4

HCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 540230723-Ethoxy-2-(p-butylphenyl)acroleinHCID 178444523HCID 178444523、化合物

生成物 1

HCID 178444383HCID 178444383、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

In an analogous manner to that described in Example 3, a mixture of 6.3 g of 3-ethoxy-2-(p-butylphenyl)acrolein, 6.6 g of trans-4-pentylcyclohexanecarboxamidine hydrochloride and 60 ml of absolute methanol is treated with a sodium methylate solution prepared from 1.1 g of sodium in 25 ml of absolute methanol. The reaction duration, working-up and chromatography are as described in Example 3. The pure fractions (in accordance with thin-layer chromatography) resulting in the chromatography are combined and recrystallized twice from hexane. There is obtained analytically pure trans-2-(4-pentylcyclohexyl)-5-(p-butylphenyl)pyrimidine; m.p. 87° C., smectic-nematic phase transition 136.5° C., cl.p. 146.5° C.

後処理

  1. customThe pure fractions (in accordance with thin-layer chromatography) resulting in the chromatography
  2. customrecrystallized twice from hexane

出典と根拠

ORDレコード
ord-2afb3376875248f685d6e49e951e8bc1
出典データセット
uspto-grants-1984_07
特許番号
US04462923

反応ノート

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