Triethylamine → HCID 67958192, 화합물

HRID 72511

반응식

HRID 72511 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH:9]2[CH2:12][NH:11][CH2:10]2)=[C:4]([CH3:13])[CH:3]=1.C(N(CC)CC)C.Cl[C:22]1[N:43]=[CH:42][C:41]([Cl:44])=[CH:40][C:23]=1[C:24]([NH:26][C:27]1([C:30]2[CH:39]=[CH:38][C:33]([C:34]([O:36][CH3:37])=[O:35])=[CH:32][CH:31]=2)[CH2:29][CH2:28]1)=[O:25]>O1CCCC1.CO>[Cl:44][C:41]1[CH:42]=[N:43][C:22]([N:11]2[CH2:12][CH:9]([NH:8][C:5]3[CH:6]=[CH:7][C:2]([F:1])=[CH:3][C:4]=3[CH3:13])[CH2:10]2)=[C:23]([CH:40]=1)[C:24]([NH:26][C:27]1([C:30]2[CH:31]=[CH:32][C:33]([C:34]([O:36][CH3:37])=[O:35])=[CH:38][CH:39]=2)[CH2:29][CH2:28]1)=[O:25]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 65958632N-(4-fluoro-2-methylphenyl)azetidin-3-amineHCID 86697873Methyl 4-(1-(2,5-dichloronicotinamido)cyclopropyl)benzoate

생성물 1

HCID 67958192HCID 67958192, 화합물

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

반응 조건

온도
75 °C

실험 절차

To a solution of N-(4-fluoro-2-methylphenyl)azetidin-3-amine (D55) and triethylamine (0.14 ml, 1.04 mmol) in tetrahydrofuran/methanol (3 ml/1 ml) methyl 4-(1-(2,5-dichloronicotinamido)cyclopropyl)benzoate (D97) (253 mg, 0.693 mmol) was added and the resulting mixture was heated 24 h at 75° C. The residue obtained after solvent evaporation, was purified by Biotage SNAP-Si (10 g) cartridge eluting with eluting with a mixture dichloromethane/ethylacetate from 95/5 to 80/20. Collected fractions, after solvent evaporation afforded the title compound (D168) (105 mg).

후처리

  1. customThe residue obtained
  2. customafter solvent evaporation
  3. customwas purified by Biotage SNAP-Si (10 g) cartridge
  4. washeluting
  5. washwith eluting with a mixture dichloromethane/ethylacetate from 95/5 to 80/20
  6. customCollected fractions, after solvent evaporation

출처 및 근거

ORD 기록
ord-087db1940e3d4e408bbd2d90170e5faf
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08828987B2

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