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Water → HCID 46198823, 화합물

HRID 1930599
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HRID 1930599 반응식
[F:1][C:2]1[CH:33]=[CH:32][C:5]([CH2:6][C:7]2[C:8]3[CH2:31][S:30][CH2:29][CH2:28][C:9]=3[N:10]=[C:11]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([N:20]4[CH:24]=[C:23]([CH3:25])[N:22]=[CH:21]4)=[C:16]([O:26][CH3:27])[CH:15]=3)[N:12]=2)=[CH:4][CH:3]=1.ClC1C=CC=C(C(OO)=[O:42])C=1.C([O-])(O)=O.[Na+].O>C(Cl)Cl>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][C:7]2[C:8]3[CH2:31][S:30](=[O:42])[CH2:29][CH2:28][C:9]=3[N:10]=[C:11]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([N:20]4[CH:24]=[C:23]([CH3:25])[N:22]=[CH:21]4)=[C:16]([O:26][CH3:27])[CH:15]=3)[N:12]=2)=[CH:32][CH:33]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 593338014-(4-Fluorobenzyl)-N-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-7,8-dihydro-5H-thiopyrano[4,3-d]pyrimidin-2-amine

생성물 1

HCID 46198823HCID 46198823, 화합물수율 18.7%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

4-(4-Fluorobenzyl)-N-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-7,8-dihydro-5H-thiopyrano[4,3-d]pyrimidin-2-amine (254 mg, 0.55 mmol) and meta-chloroperbenzoic acid (95 mg, 0.55 mmol) was slurrified in DCM (4 mL). Saturated NaHCO3 and water were added to the reaction mixture, the organic phase was separated and the solvent was evaporated. The crude product was purified on preparative HPLC yielding 4-(4-fluorobenzyl)-N-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]-7,8-dihydro-5H-thiopyrano[4,3-d]pyrimidin-2-amine 6-oxide (49.0 mg, 18%).

후처리

  1. customthe organic phase was separated
  2. customthe solvent was evaporated
  3. customThe crude product was purified on preparative HPLC

출처 및 근거

ORD 기록
ord-3787774c5e9f4a0a9823204514aa9be1
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08188101B2

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