Dichloromethane → (E)-3-[4-(2-Morpholin-4-yl-ethyl)-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl]acrylic acid hydrochloride
反応式
C([O:5][C:6](=[O:29])/[CH:7]=[CH:8]/[C:9]1[CH:28]=[N:27][C:12]2[NH:13][C:14](=[O:26])[CH2:15][N:16]([CH2:18][CH2:19][N:20]3[CH2:25][CH2:24][O:23][CH2:22][CH2:21]3)[CH2:17][C:11]=2[CH:10]=1)(C)(C)C.C(O)(C(F)(F)F)=O.C(Cl)[Cl:38]>>[ClH:38].[N:20]1([CH2:19][CH2:18][N:16]2[CH2:17][C:11]3[CH:10]=[C:9](/[CH:8]=[CH:7]/[C:6]([OH:29])=[O:5])[CH:28]=[N:27][C:12]=3[NH:13][C:14](=[O:26])[CH2:15]2)[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1参加物
4
反応物 3
生成物 1
実験手順
A solution of (E)-3-[4-(2-morpholin-4-yl-ethyl)-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl]acrylic acid tert-butyl ester (92 mg, 0.23 mmol) in CH2Cl2 (2 mL) was treated with TFA (2 mL). After stirring at room temperature for 30 min, the clear tan solution was concentrated in vacuo. The resulting oil was treated with anhydrous HCl (4 mL of a 4.0 M solution in dioxane, 16 mmol) and then sonicated for 15 min. The mixture was diluted with Et2O and sonicated for 10 min. The solid was isolated by filtration, washed with Et2O and dried under vacuum at 50° C. for 4.5 hr to give the title compound (0.10 g, 96%) as an off-white solid: MS (ESI) m/e 347 (M+H)+.
後処理
- concentrationthe clear tan solution was concentrated in vacuo
- additionThe resulting oil was treated with anhydrous HCl (4 mL of a 4.0 M solution in dioxane, 16 mmol) and
- customthen sonicated for 15 min
- additionThe mixture was diluted with Et2O
- customsonicated for 10 min
- customThe solid was isolated by filtration
- washwashed with Et2O
- customdried under vacuum at 50° C. for 4.5 hr
出典と根拠
- ORDレコード
- ord-ed8c825313404d86bb7d0373458041e8
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07879872B2
反応ノート
読み込み中…