1,3-Difluoro-5-isocyanatobenzene → HCID 90266348, 화합물

HRID 631841

반응식

HRID 631841 반응식
[F:1][C:2]1[CH:7]=[C:6]([N:8]=[C:9]=[O:10])[CH:5]=[C:4]([F:11])[CH:3]=1.[F:12][C:13]1[C:14](=[NH:21])[N:15]([CH3:20])[C:16](=[O:19])[NH:17][CH:18]=1>CN(C=O)C>[F:1][C:2]1[CH:7]=[C:6]([NH:8][C:9]([N:17]2[CH:18]=[C:13]([F:12])[C:14](=[NH:21])[N:15]([CH3:20])[C:16]2=[O:19])=[O:10])[CH:5]=[C:4]([F:11])[CH:3]=1

참가 물질

4

반응물 2

HCID 27792821,3-Difluoro-5-isocyanatobenzeneHCID 178481639HCID 178481639, 화합물

생성물 1

HCID 90266348HCID 90266348, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1,3-Difluoro-5-isocyanatobenzene (119 mg, 0.769 mmol) was added to a solution of 5-fluoro-4-imino-3-methyl-3,4-dihydropyrimidin-2(1H)-one (100 mg, 0.699 mmol) in DMF (1.8 mL) and stirred overnight at room temperature. The solution was then concentrated under vacuum and the resulting residue stirred in dichloromethane (2 mL) for 30 min. The solids were filtered and washed with dichloromethane (2×3 mL) and dried under vacuum to afford the title compound; mp 203.0-204.5° C.; 1H NMR (400 MHz, CDCl3) δ 11.03 (s, 1H), 9.87 (s, 1H), 7.68 (d, J=6.2 Hz, 1H), 7.25 (d, J=7.4 Hz, 2H), 6.80 (s, 1H), 3.25 (s, 3H); 13C NMR (101 MHz, DMSO-d6) δ 163.77, 163.62, 161.36, 161.21, 158.57, 149.14, 146.14, 145.90, 142.72, 142.58, 142.44, 138.68, 136.41, 122.85, 122.52, 101.05, 100.76, 97.32, 97.06, 96.79, 29.43; ESIMS m/z 299.0 ([M+H]+).

후처리

  1. concentrationThe solution was then concentrated under vacuum
  2. stirringthe resulting residue stirred in dichloromethane (2 mL) for 30 min
  3. filtrationThe solids were filtered
  4. washwashed with dichloromethane (2×3 mL)
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-7ec31520f4b34247abd0985fff98ba0e
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321734B2

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