Acetic Anhydride → HCID 178474341, 화합물
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[NH2:1][C:2]1[CH:6]=[CH:5][NH:4][N:3]=1.C([O-])(O)=O.[Na+].[CH3:12][C:13](OC(C)=O)=[O:14]>O>[NH:4]1[CH:5]=[CH:6][C:2]([NH:1][C:13](=[O:14])[CH3:12])=[N:3]1참가 물질
5
실험 절차
To a solution of 3-aminopyrazole (20 g, 0.24 mol) in H2O (36 mL), at 5-10° C., was slowly added NaHCO3 (9.1 g, mol, 3 eq) and then Ac2O (6.79 ml, 2 eq). The reaction mixture was refluxed for 8 hr. It was cooled down to r.t. and was left standing at this temperature for 12 hr to allow crystallization. The white solid was filtered (12.9 g) and the mother liquor volume was reduced. A second batch of white solid (3.4 g) was obtained after crystallization. The two batches were combined to give the title compound (16.3 g, 54%).
후처리
- customat 5-10° C.
- temperatureThe reaction mixture was refluxed for 8 hr
- waitwas left
- customcrystallization
- filtrationThe white solid was filtered (12.9 g)
출처 및 근거
- ORD 기록
- ord-d8cc33e5f25f40949a2c7f8221c44612
- 출처 데이터셋
- uspto-grants-2008_09
- 특허 번호
- US07427630B2
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