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6-Chloro-N-(4-(methylsulfonyl)phenyl)-5-nitropyrimidin-4-amine → HCID 21897803, 화합물

HRID 719520
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HRID 719520 반응식
[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:11][CH:10]=2)[C:3]=1[N+:19]([O-])=O.[N:22]([O-])=O.[Na+]>ClCCl.C(O)(=O)C.O>[Cl:1][C:2]1[C:3]2[N:19]=[N:22][N:8]([C:9]3[CH:14]=[CH:13][C:12]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:11][CH:10]=3)[C:4]=2[N:5]=[CH:6][N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 218978866-Chloro-N-(4-(methylsulfonyl)phenyl)-5-nitropyrimidin-4-amineHCID 23668193Sodium Nitrite

생성물 1

HCID 21897803HCID 21897803, 화합물수율 77.8%

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 962Water용매HCID 6344Dichloromethane
용매

실험 절차

To a solution of (6-chloro-5-nitro-pyrimidin-4-yl)-(4-methanesulfonyl-phenyl)-amine in dichloromethane (8 mL) and 50% aqueous acetic acid (6 mL) was added sodium nitrite (64.6 mg, 0.937 mmol) in water (1 mL) dropwise at room temperature. After the addition was complete, the reaction was stirred for additional 15 minutes at room temperature. The organic layer was then separated, washed with water, and dried over anhydrous magnesium sulfate. Filtration followed by removal of volatiles under high vacuum afforded the desired product as a yellow solid (205 mg, 77.8%).

후처리

  1. additionAfter the addition
  2. customThe organic layer was then separated
  3. washwashed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationFiltration
  6. customfollowed by removal of volatiles under high vacuum

출처 및 근거

ORD 기록
ord-f3bc561decfd44b2821a43bc22e686bc
출처 데이터셋
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07132426B2

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