반응식
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[CH:19]=[CH:18][C:15]([CH:16]=O)=[CH:14][CH:13]=2)=[O:11])[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[NH:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].[OH-].[Na+]>C1COCC1>[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[CH:19]=[CH:18][C:15]([CH2:16][N:20]3[CH2:25][CH2:24][O:23][CH2:22][CH2:21]3)=[CH:14][CH:13]=2)=[O:11])[CH2:6][CH2:5]1)([CH3:3])[CH3:2]참가 물질
실험 절차
To a solution of 4-(4-isopropyl-piperazine-1-carbonyl)-benzaldehyde (4.0 g, 15.38 mmol) in THF (40 mL) was added morpholine (2.9 g, 33.83 mmol), and the resulting mixture was stirred at room temperature for 1 h before it was cooled to 0° C. with an ice bath. The reaction mixture was then treated with NaBH(OAc)3 (4.56 g, 21.53 mmol) in portions over 15 min. The resulting suspension was stirred at room temperature until it was deemed complete by HPLC. After completion, 10% NaOH (25 mL) was added and the reaction was vigorously agitated for 15 min. The phases were separated and the aqueous layer was extracted with THF (20 mL). The organic layers were combined, dried (MgSO4), filtered and concentrated to yield the title compound as a yellow oil.
후처리
- temperaturewas cooled to 0° C. with an ice bath
- stirringThe resulting suspension was stirred at room temperature until it
- stirringthe reaction was vigorously agitated for 15 min
- customThe phases were separated
- extractionthe aqueous layer was extracted with THF (20 mL)
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-578d972b992f4013ac9230ab24fabcf8
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07728129B2
연결된 노트
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