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Hexane → HCID 66977211, 화합물

HRID 712230
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HRID 712230 반응식
Cl.[F:2][C:3]([F:14])([F:13])[C:4]1([C:9]([O:11][CH3:12])=[O:10])[CH2:8][CH2:7][NH:6][CH2:5]1.CCN(C(C)C)C(C)C.[Br:24][C:25]1[CH:26]=[N:27][C:28](Cl)=[N:29][CH:30]=1.CCCCCC>CCO>[Br:24][C:25]1[CH:26]=[N:27][C:28]([N:6]2[CH2:7][CH2:8][C:4]([C:3]([F:2])([F:13])[F:14])([C:9]([O:11][CH3:12])=[O:10])[CH2:5]2)=[N:29][CH:30]=1
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참가 물질

6

반응물 4

HCID 8058HexaneHCID 81531DiisopropylethylamineHCID 6066655-Bromo-2-chloropyrimidineHCID 66976916Methyl 3-(trifluoromethyl)pyrrolidine-3-carboxylate hydrochloride

생성물 1

HCID 66977211HCID 66977211, 화합물수율 63%

시약·촉매·용매 1

HCID 702Ethanol
용매

실험 절차

To a solution of methyl 3-(trifluoromethyl)pyrrolidine-3-carboxylate hydrochloride (0.32 g, 1.36 mmol) in EtOH (10.0 mL) was added DIPEA (1.1 mL, 6.79 mmol) at rt and the mixture stirred at rt for 10 min followed by addition of 5-bromo-2-chloropyrimidine (0.26 g, 1.36 mmol). The reaction was heated up to 70° C. for 1 h. After reaction completion (by TLC), the solvent was evaporated and the crude residue purified over 60-120 M silica-gel using 10.0% EtOAc:hexane to obtain the desired product as a yellow solid (0.30 g, 63% yield). MS: 354.02 [M+H]+.

후처리

  1. temperatureThe reaction was heated up to 70° C. for 1 h
  2. customAfter reaction completion (by TLC)
  3. customthe solvent was evaporated
  4. customthe crude residue purified over 60-120 M silica-gel

출처 및 근거

ORD 기록
ord-94dcfc86a5f44c47b1a50da24678a3e3
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181234B2

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