HCID 23103622、化合物 → HCID 23103618、化合物

HRID 2116507ノート

反応式

HRID 2116507 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]([C:11]2[CH:12]=[C:13](Cl)[N:14]=[N:15][C:16]=2[O:17][CH3:18])[OH:10])=[CH:5][CH:4]=1)[CH3:2].C(C1C=CC(C(C2[CH:35]=[C:34]([O:36]C)N=NC=2Cl)O)=CC=1)C>[Pd].C(O)(=O)C>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:11]2[CH:12]=[CH:13][N:14]=[N:15][C:16]=2[O:17][CH3:18])=[CH:5][CH:4]=1)[CH3:2].[C:34]([OH:36])(=[O:10])[CH3:35].[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:11]2[CH:12]=[CH:13][N:14]=[N:15][C:16]=2[O:17][CH3:18])=[CH:5][CH:4]=1)[CH3:2]

参加物

6

反応物 2

HCID 23103622HCID 23103622、化合物HCID 23103633HCID 23103633、化合物

生成物 2

HCID 23103618HCID 23103618、化合物HCID 69220153HCID 69220153、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

The 6:1 mixture of (4-ethylphenyl)-(3-chloro-6-methoxypyridazin-5-yl)-methanol and (4-ethylphenyl)-(3-chloro-6-methoxypyridazin-4-yl)-methanol (10.7 g), 5% palladium/carbon (5.4 g) and acetic acid (80 ml) were suspended and stirred under a hydrogen atmosphere at room temperature for 22 hours. After filtration to remove the insoluble materials, the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:2 to chloroform:methanol=10:1) to give 4-(4-ethylbenzyl)-3-methoxy-pyridazine (2.88 g) and 4-(4-ethylbenzyl)-3-methoxy-pyridazine acetate salt (3.32 g).

後処理

  1. filtrationAfter filtration
  2. customto remove the insoluble materials
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customthe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:2 to chloroform:methanol=10:1)

出典と根拠

ORDレコード
ord-2fafe29db2d94770a5aa1b0b7115cf5c
出典データセット
uspto-grants-2008_10
特許番号
US07439232B2

反応ノート

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