Diisopropylethylamine → HCID 10273764、化合物

HRID 1635853ノート

反応式

HRID 1635853 の反応式
[CH:1]1[CH:2]=[CH:3][N:4]2[CH2:10][C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[NH:7][CH2:6][C:5]=12.C(N(C(C)C)CC)(C)C.[F:24][C:25]([F:41])([F:40])[C:26]1[CH:30]=[CH:29][N:28]([C:31]2[CH:39]=[CH:38][C:34]([C:35](Cl)=[O:36])=[CH:33][CH:32]=2)[N:27]=1>ClCCl>[CH:1]1[CH:2]=[CH:3][N:4]2[CH2:10][C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[N:7]([C:35]([C:34]3[CH:33]=[CH:32][C:31]([N:28]4[CH:29]=[CH:30][C:26]([C:25]([F:41])([F:24])[F:40])=[N:27]4)=[CH:39][CH:38]=3)=[O:36])[CH2:6][C:5]=12

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 27807004-[3-(trifluoromethyl)-1H-pyrazol-1-yl]benzoyl chlorideHCID 1554704810,11-Dihydro-5H-benzo[e]pyrrolo[1,2-a][1,4]diazepine

生成物 1

HCID 10273764HCID 10273764、化合物収率 84.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]-benzodiazepine (0.88 g) and diisopropylethylamine (0.66 g) in dichloromethane (50 ml) was added the 4-(3-trifluoromethylpyrazol-1-yl)benzoyl chloride (1.40 g). After stirring at room temperature for 18 hours, the reaction mixture was washed with water and saturated aqueous sodium bicarbonate. The dichloromethane solution was dried over anhydrous sodium sulfate and filtered through a short column of hydrous sodium magnesium silicate and further eluted with several volumes of dichloromethane. The combined organic phase was concentrated on a hot plate with the gradual addition of hexane until crystallization occurred. After cooling, the crystals were collected by filtration to yield the title compound (1.70 g), m.p. 166-167° C.; MS, m/z: 423.3 (M+H)+, 845.4 (2M+H)+.

後処理

  1. washthe reaction mixture was washed with water and saturated aqueous sodium bicarbonate
  2. dry with materialThe dichloromethane solution was dried over anhydrous sodium sulfate
  3. filtrationfiltered through a short column of hydrous sodium magnesium silicate
  4. washfurther eluted with several volumes of dichloromethane
  5. concentrationThe combined organic phase was concentrated on a hot plate with the gradual addition of hexane until crystallization
  6. temperatureAfter cooling
  7. filtrationthe crystals were collected by filtration

出典と根拠

ORDレコード
ord-704277415c82455ab4a7b45c3aa2528a
出典データセット
uspto-grants-2003_01
特許番号
US06511974B1

反応ノート

読み込み中…