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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetyl chloride → HCID 57940700, 화합물

HRID 1437308
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HRID 1437308 반응식
C(N(CC)CC)C.[C:8](Cl)(=[O:10])[CH3:9].[CH3:12][O:13][C:14]1[N:19]=[CH:18][C:17]([N:20]2[C:24]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=3)=[CH:23][C:22]([C:31]([N:33]3[CH2:38][CH2:37][CH2:36][CH2:35][NH:34]3)=[O:32])=[N:21]2)=[CH:16][CH:15]=1>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH3:12][O:13][C:14]1[N:19]=[CH:18][C:17]([N:20]2[C:24]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=3)=[CH:23][C:22]([C:31]([N:33]3[CH2:38][CH2:37][CH2:36][CH2:35][N:34]3[C:8](=[O:10])[CH3:9])=[O:32])=[N:21]2)=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 11674985HCID 11674985, 화합물

생성물 1

HCID 57940700HCID 57940700, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

Triethylamine (0.210 mL), acetyl chloride (0.0807 mL) and 4-dimethylaminopyridine (13.5 mg) were added to 1-[1-(6-methoxy-3-pyridyl)-5-(2-pyridyl)pyrazole-3-carbonyl]hexahydropyridazine (0.275 g) obtained in Example 162 in methylene chloride (6.0 mL) at room temperature, followed by stirring for 20 minutes. The mixture was partitioned between water and chloroform. The organic layer was washed with saturated brine, and then dried over sodium sulfate anhydrate. The mixture was subjected to filtration, and the solvent was removed under reduced pressure. The residue was purified through silica gel column chromatography (chloroform-methanol), to thereby give the title compound as an amorphous product (0.149 g, 59%).

후처리

  1. customThe mixture was partitioned between water and chloroform
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over sodium sulfate anhydrate
  4. filtrationThe mixture was subjected to filtration
  5. customthe solvent was removed under reduced pressure
  6. customThe residue was purified through silica gel column chromatography (chloroform-methanol)

출처 및 근거

ORD 기록
ord-8a17b77d638f45a3a1b6f6114b955e90
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07622471B2

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