Ammonia → HCID 86687002, 화합물
반응식
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]=1참가 물질
7
반응 조건
- 온도
- 160 °C
실험 절차
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+].
후처리
- washwashed with MeOH
- washThe product was eluted with 2M NH3 in MeOH
- concentrationconcentration in vacuo
- customgave a residue
출처 및 근거
- ORD 기록
- ord-3901212e33fc43cf98ec082c3768565b
- 출처 데이터셋
- uspto-grants-2015_09
- 특허 번호
- US09145413B2
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