Triethylamine → 1-(4-(4-(2-tert-butyl-6-(trifluoromethyl)pyrimidin-4-yl)piperazin-1-yl)butyl)-3,4-dihydro-1H-benzo[b]azepine-2,5-dione

HRID 2240618노트

반응식

HRID 2240618 반응식
Cl[CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[C:10](=[O:17])[CH2:9][CH2:8][C:7]1=[O:18].[C:19]([C:23]1[N:28]=[C:27]([N:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)[CH:26]=[C:25]([C:35]([F:38])([F:37])[F:36])[N:24]=1)([CH3:22])([CH3:21])[CH3:20].C(N(CC)CC)C.C(OCC)(=O)C>CN(C)C=O>[C:19]([C:23]1[N:28]=[C:27]([N:29]2[CH2:30][CH2:31][N:32]([CH2:2][CH2:3][CH2:4][CH2:5][N:6]3[C:12]4[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=4[C:10](=[O:17])[CH2:9][CH2:8][C:7]3=[O:18])[CH2:33][CH2:34]2)[CH:26]=[C:25]([C:35]([F:36])([F:37])[F:38])[N:24]=1)([CH3:22])([CH3:20])[CH3:21]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 183996102-(tert-Butyl)-4-(piperazin-1-yl)-6-(trifluoromethyl)pyrimidineHCID 685828961-(4-chlorobutyl)-3,4-dihydro-1H-benzo[b]azepine-2,5-dione

생성물 1

HCID 112376641-(4-(4-(2-tert-butyl-6-(trifluoromethyl)pyrimidin-4-yl)piperazin-1-yl)butyl)-3,4-dihydro-1H-benzo[b]azepine-2,5-dione

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1-(4-Chlorobutyl)-3,4-dihydro-1H-1-benzazepine-2,5-dione (3.29 mmol, 1.75 g, 70%), 2-tert-butyl-4-piperazin-1-yl-6-(trifluoromethyl)pyrimidine (3.56 mmol, 1.03 g; preparation according to WO 99/02503) and triethylamine (13.17 mmol, 1.33 g) in dimethylformamide (100 ml) were stirred at 100° C. for 12 h. Afterward, ethyl acetate was added and the mixture was washed twice with water. The combined organic phases were dried over Na2SO4, filtered and concentrated under reduced pressure. The oily residue was purified by chromatography on silica gel (eluent: 95:5 v/v dichloromethane:methanol); yield 0.42 g.

후처리

  1. washthe mixture was washed twice with water
  2. dry with materialThe combined organic phases were dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe oily residue was purified by chromatography on silica gel (eluent: 95:5 v/v dichloromethane:methanol)

출처 및 근거

ORD 기록
ord-4d80c3045ad24eba800debbc36eac546
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07723384B2

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