반응식
CCN=C=NCCCN(C)C.[CH2:12]([N:14]1[C:18]([C:19]2[CH:20]=[C:21]([C:32](O)=[O:33])[CH:22]=[C:23]([C:25]3[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][CH:26]=3)[CH:24]=2)=[N:17][N:16]=[N:15]1)[CH3:13].C1C=CC2N(O)N=NC=2C=1.CN1C(=O)CCC1.[CH3:52][O:53][CH2:54][CH:55]([NH2:57])[CH3:56]>C(Cl)Cl>[CH3:52][O:53][CH2:54][CH:55]([NH:57][C:32]([C:21]1[CH:22]=[C:23]([C:25]2[CH:26]=[CH:27][C:28]([CH3:31])=[CH:29][CH:30]=2)[CH:24]=[C:19]([C:18]2[N:14]([CH2:12][CH3:13])[N:15]=[N:16][N:17]=2)[CH:20]=1)=[O:33])[CH3:56]참가 물질
7
반응물 5
생성물 1
시약·촉매·용매 1
실험 절차
EDCI (54.0 mg, 0.282 mmol) was added in one portion to a solution of 5-(1-ethyl-1H-tetrazol-5-yl)-4′-methyl-biphenyl-3-carboxylic acid (70.0 mg, 0.229 mmol), HOBt (40.0 mg, 0.296 mmol) and NMP (101.5 mg, 1.000 mmol) in CH2Cl2 (5 mL) at 0° C. After the reaction stirred at the same temperature for 1 hour, 2-methoxy-1-methyl-ethylamine (64.3 mg, 0.72 mmol) was added. The mixture was allowed to warm to room temperature and was stirred overnight. Solvent was removed under reduced pressure and the residue was purified by column chromatography to afford 5-(1-ethyl-1H-tetrazol-5-yl)-4′-methyl-biphenyl-3-carboxylic acid (2-methoxy-1-methyl-ethyl)-amide as white solid (40 mg, 46%). MS (M+H)=380.
후처리
- stirringwas stirred overnight
- customSolvent was removed under reduced pressure
- customthe residue was purified by column chromatography
출처 및 근거
- ORD 기록
- ord-a58e4ad2b5924bc39348acbe1fb1c5d0
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08846945B2
연결된 노트
불러오는 중…