1-[4-(4-Benzyloxyphenyl)butyl]-1,2,4-triazole → 1-[4-(4-Hydroxyphenyl)butyl]-1,2,4-triazole

HRID 322256ノート

反応式

HRID 322256 の反応式
C([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][CH2:17][CH2:18][N:19]2[CH:23]=[N:22][CH:21]=[N:20]2)=[CH:11][CH:10]=1)C1C=CC=CC=1>[C].[Pd].C(O)C>[OH:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][CH2:17][CH2:18][N:19]2[CH:23]=[N:22][CH:21]=[N:20]2)=[CH:11][CH:10]=1

参加物

4

実験手順

A mixture of 1-[4-(4-benzyloxyphenyl)butyl]-1,2,4-triazole (3.15 g), palladium-carbon (5%, 3.0 g) and ethanol (50 ml) was subjected to catalytic hydrogenation under atmospheric pressure at room temperature. The catalyst was filtered off, and the filtrate was concentrated. The residue was subjected to a silica gel column chromatography. The crystalline product obtained from the fraction eluted with tetrahydrofuran-hexane (1:1, v/v) was recrystallized from ethyl acetate-hexane to give 1-[4-(4-hydroxyphenyl)butyl]-1,2,4-triazole (1.22 g, 55%) as colorless prisms, mp 135-136° C.

後処理

  1. customwas subjected to catalytic hydrogenation under atmospheric pressure at room temperature
  2. filtrationThe catalyst was filtered off
  3. concentrationthe filtrate was concentrated
  4. customThe crystalline product obtained from the fraction
  5. washeluted with tetrahydrofuran-hexane (1:1
  6. customv/v) was recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-48e1fa762fb7461fb53c2c44b99a5ac7
出典データセット
uspto-grants-2001_04
特許番号
US06211215B1

反応ノート

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