HCID 23103622, 화합물 → HCID 23103618, 화합물

HRID 2116507노트

반응식

HRID 2116507 반응식
[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]

참가 물질

6

반응물 2

HCID 23103622HCID 23103622, 화합물HCID 23103633HCID 23103633, 화합물

생성물 2

HCID 23103618HCID 23103618, 화합물HCID 69220153HCID 69220153, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-2fafe29db2d94770a5aa1b0b7115cf5c
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07439232B2

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