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Carbon Tetrachloride → tert-Butyl 4-chloro-2-(trifluoromethyl)-5,8-dihydropyrido[3,4-d]pyrimidine-7(6H)-carboxylate

HRID 2406218
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HRID 2406218 반응식
O[C:2]1[C:3]2[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][C:4]=2[N:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[N:7]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:43]>ClC(Cl)C>[Cl:43][C:2]1[C:3]2[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][C:4]=2[N:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[N:7]=1
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참가 물질

5

반응물 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 178451641HCID 178451641, 화합물

생성물 1

HCID 71742291tert-Butyl 4-chloro-2-(trifluoromethyl)-5,8-dihydropyrido[3,4-d]pyrimidine-7(6H)-carboxylate수율 96.3%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

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온도
70 °C

실험 절차

tert-Butyl 4-hydroxy-2-(trifluoromethyl)-5,6-dihydropyrido[3,4-d]pyrimidine-7(8H)-carboxylate (5.12 g, 16.05 mmol) was combined with triphenylphosphine (8.42 g, 32.1 mmol) and stirred in dichloroethane (160 mL) at ambient temperature for 15 minutes, and then carbon tetrachloride (7.41 g, 48.1 mmol) was added. The reaction was stirred at 70° C. for 3 hours, cooled to room temperature, and concentrated in vacuo. The crude residue was purified by flash chromatography on silica gel (elution gradient from 0% to 3% methanol/DCM) to afford the title compound as a clear oil (5.22 g, 86% yield). MS (ESI) m/e (M−H)−=336.3.

후처리

  1. temperaturecooled to room temperature
  2. concentrationconcentrated in vacuo
  3. customThe crude residue was purified by flash chromatography on silica gel (elution gradient from 0% to 3% methanol/DCM)

출처 및 근거

ORD 기록
ord-05e6356bac254c7a82f80c0a215903bf
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809352B2

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