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Phenyl chloroformate → HCID 67295418, 화합물

HRID 629019
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HRID 629019 반응식
Cl[C:2]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:3].[CH3:11][S:12][C:13]1[C:14]([N:26]2[CH2:31][CH2:30][O:29][CH2:28][CH2:27]2)=[N:15][C:16]([C:19]2[CH:24]=[CH:23][C:22]([NH2:25])=[CH:21][CH:20]=2)=[N:17][CH:18]=1.C([O-])(O)=O.[Na+]>C(#N)C>[CH3:11][S:12][C:13]1[C:14]([N:26]2[CH2:31][CH2:30][O:29][CH2:28][CH2:27]2)=[N:15][C:16]([C:19]2[CH:24]=[CH:23][C:22]([NH:25][C:2](=[O:3])[O:4][C:5]3[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=3)=[CH:21][CH:20]=2)=[N:17][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 15891Phenyl chloroformateHCID 516892Sodium BicarbonateHCID 67295403HCID 67295403, 화합물

생성물 1

HCID 67295418HCID 67295418, 화합물수율 80%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

The phenyl chloroformate (0.84 ml, 6.68 mmole, 2.5 eq) was added to a mixture of 4-(5-(methylthio)-4morpholinopyrimidin-2-yl)benzeneamine (0.84 g, 2.18 mmole, 1 eq), NaHCO3(aq) (1M, 6.3 ml, 6.3 mmole 2.2 eq) and ACN (13 ml) at 0□. The reaction mixture was stirred for 8 hrs and then dried. The reaction mixture was partitioned between EA and water, the organic layer was washed with brine, dried over MgSO4, filtered and evaporated in vacuo. The resulting residue was purified by flash chromatography on silica gel (Hexane/EtOAc 2:1) to give a yellow solid (80%).

후처리

  1. customdried
  2. customThe reaction mixture was partitioned between EA and water
  3. washthe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customThe resulting residue was purified by flash chromatography on silica gel (Hexane/EtOAc 2:1)

출처 및 근거

ORD 기록
ord-6d17f00d434f4dcd95207c23f26fb8ee
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09315491B2

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