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Acetic Anhydride → HCID 69709723, 화합물

HRID 392106
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HRID 392106 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:10]2[CH2:22][NH:21][CH2:20][CH2:19][C:11]=2[N:12]=[C:13]([S:15]([CH3:18])(=[O:17])=[O:16])[N:14]=1.C(N(CC)CC)C.[C:30](OC(=O)C)(=[O:32])[CH3:31]>ClCCl>[C:30]([N:21]1[CH2:20][CH2:19][C:11]2[N:12]=[C:13]([S:15]([CH3:18])(=[O:17])=[O:16])[N:14]=[C:9]([C:3]3[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=3[Cl:1])[C:10]=2[CH2:22]1)(=[O:32])[CH3:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 69710990HCID 69710990, 화합물

생성물 1

HCID 69709723HCID 69709723, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-(2,4-dichlorophenyl)-2-(methylsulfonyl)-5,6,7,8-tetrahydropyridino[4,3-d]pyrimidine (100 mg, 0.279 mmol), triethylamine (78 μl, 0.558 mmol) in dichloromethane (2 ml) was added acetic anhydride (53 μl, 0.558 mmol) dropwise. The resulting mixture was stirred at room temperature overnight. The mixture was partitioned between ethyl acetate and water. Organic layer was separated and washed with brine, dried (MgSO4) and filtered. Concentration of filtrate afforded crude product 6-acetyl-4-(2,4-dichlorophenyl)-2-(methylsulfonyl)-5,6,7,8-tetrahydropyridino[4,3-d]pyrimidine in quantitative yield.

후처리

  1. customThe mixture was partitioned between ethyl acetate and water
  2. customOrganic layer was separated
  3. washwashed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-6c43cd192cdb4762b155fd542d30d239
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06800632B2

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