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 2240618ノート

反応式

HRID 2240618 の反応式
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]

参加物

6

反応物 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

生成物 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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-4d80c3045ad24eba800debbc36eac546
出典データセット
uspto-grants-2010_05
特許番号
US07723384B2

反応ノート

読み込み中…