Ammonia → 3-Amino-2-chlorobenzamide
반응식
[NH2:1][C:2]1[C:3]([Cl:11])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5](O)=[O:6].CC[N:14](C(C)C)C(C)C.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.N>C(Cl)Cl.O.CCOC(C)=O>[NH2:1][C:2]1[C:3]([Cl:11])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([NH2:14])=[O:6]참가 물질
9
실험 절차
To a solution of 3-amino-2-chlorobenzoic acid (5.8 mmol) in 12 mL DCM were added 3.0 mL DIPEA, HOBT (7.0 mmol) and EDC.HCl (7.0 mmol) followed by the addition of 0.67 mL of a solution of NH3 in water (13M). The mixture was stirred at RT overnight, EtOAc was then added and the mixture was extracted with water, sat. aq. NaHCO3 solution and brine. The organic layer was dried over MgSO4 and concentrated in vacuo to obtain the desired compound as yellow solid.
후처리
- extractionthe mixture was extracted with water, sat. aq. NaHCO3 solution and brine
- dry with materialThe organic layer was dried over MgSO4
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-94310c0c15f946ef87d7511c86cc4499
- 출처 데이터셋
- uspto-grants-2015_12
- 특허 번호
- US09221832B2
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