Sodium → HCID 178444383, 화합물

HRID 1463013

반응식

HRID 1463013 반응식
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]

참가 물질

6

반응물 4

HCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 54023072HCID 54023072, 화합물HCID 178444523HCID 178444523, 화합물

생성물 1

HCID 178444383HCID 178444383, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-2afb3376875248f685d6e49e951e8bc1
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04462923

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