Ammonia → HCID 86687002、化合物
反応式
Cl[C:2]1[N:6]2[CH:7]=[C:8]([F:11])[CH:9]=[CH:10][C:5]2=[N:4][N:3]=1.[NH:12]1[CH2:18][CH2:17][CH2:16][C@H:13]1[CH2:14][OH:15].N>CN1C(=O)CCC1.CO.C(Cl)Cl>[F:11][C:8]1[CH:9]=[CH:10][C:5]2[N:6]([C:2]([N:12]3[CH2:18][CH2:17][CH2:16][C@H:13]3[CH2:14][OH:15])=[N:3][N:4]=2)[CH:7]=1参加物
7
反応条件
- 温度
- 160 °C
実験手順
A mixture of Intermediate 24b (300 mg, 1.74 mmol) and L-prolinol (704 mg, 9.96 mmol) in NMP (4 mL) was heated in the microwave at 160° C. for 2 h. The reaction mixture was applied to an SCX-2 cartridge (70 g) and washed with MeOH. The product was eluted with 2M NH3 in MeOH; concentration in vacuo gave a residue. FCC, using 0-10% [2M NH3 in MeOH] in DCM, gave the title compound (210 mg, 50%). LCMS (Method 4): Rt 1.50 min, m/z 237 [MH+].
後処理
- washwashed with MeOH
- washThe product was eluted with 2M NH3 in MeOH
- concentrationconcentration in vacuo
- customgave a residue
出典と根拠
- ORDレコード
- ord-10e64a2d4a2e4402b96c4b7349ee5268
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09139584B2
反応ノート
読み込み中…