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Sodium Bicarbonate → HCID 58484971, 화합물

HRID 1255438
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HRID 1255438 반응식
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1.[F:12][C:13]1([F:27])[CH2:17][CH2:16][C@@H:15]([NH:18][CH2:19][C:20]2([C:23]([O:25][CH3:26])=[O:24])[CH2:22][CH2:21]2)[CH2:14]1.C(=O)(O)[O-].[Na+]>ClCCl>[Cl:1][C:2]1[N:7]=[C:6]([N:18]([CH2:19][C:20]2([C:23]([O:25][CH3:26])=[O:24])[CH2:22][CH2:21]2)[C@@H:15]2[CH2:16][CH2:17][C:13]([F:12])([F:27])[CH2:14]2)[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1
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참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 5212662,4-Dichloro-5-nitropyrimidineHCID 58484956HCID 58484956, 화합물

생성물 1

HCID 58484971HCID 58484971, 화합물수율 91.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

2,4-Dichloro-5-nitropyrimidine (2.16 g, 11.15 mmol) was added to a mixture of (R)-methyl 1-((3,3-difluorocyclopentylamino)methyl)cyclopropanecarboxylate (2.6 g, 11.15 mmol) and sodium bicarbonate (3.75 g, 44.64 mmol) in dichloromethane (15 mL) and petroleum ether (60 mL). The reaction mixture was stirred at room temperature for 18 hours. The reaction mixture was diluted with dichloromethane and dried over magnesium sulfate. The solids were filtered off, rinsing with more dichloromethane. The mother liquors were adsorbed on silica gel and concentrated in vacuo. The residue was purified by flash column chromatography to afford the desired product as a yellow solid (3.974 g, 91% yield).

후처리

  1. dry with materialdried over magnesium sulfate
  2. filtrationThe solids were filtered off
  3. washrinsing with more dichloromethane
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash column chromatography

출처 및 근거

ORD 기록
ord-a01b3ed5e0764ff1b2f5075ea0c30e67
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461149B2

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