반응식
[Br:1][C:2]1[CH:12]=[CH:11][C:5]([O:6][CH2:7][C:8](O)=[O:9])=[CH:4][CH:3]=1.C(Cl)(=O)C(Cl)=O.C[N:20](C=O)C>ClCCl>[Br:1][C:2]1[CH:12]=[CH:11][C:5]([O:6][CH2:7][C:8]([NH2:20])=[O:9])=[CH:4][CH:3]=1참가 물질
5
실험 절차
To a solution of (4-bromophenoxy)acetic acid (500 mg, 2.00 mmol) in dichloromethane (10 mL) and DMF (0.2 mL) was added 2M oxalyl chloride in methylene chloride (5 mL, 10 mmol). The reaction mixture was stirred at room temperature for 2 hours, and the solvent was removed under reduced pressure. Ammonium hydroxide (15 mL) was added dropwise via additional funnel. After addition, the mixture was extracted with EtOAc (3×20 mL). The combined organic layers were dried and concentrated in vacuo to give 2-(4-bromophenoxy)acetamide (350 mg, 70% yield) as a yellow solid. 1H NMR (400 MHz, CDCl3): δ 7.37-7.35 (m, 2H), 6.81-6.79 (m, 2H), 4.59 (s, 2H).
후처리
- customthe solvent was removed under reduced pressure
- additionAmmonium hydroxide (15 mL) was added dropwise via additional funnel
- additionAfter addition
- extractionthe mixture was extracted with EtOAc (3×20 mL)
- customThe combined organic layers were dried
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-0d40f7466eff4c9ca72219133632cc17
- 출처 데이터셋
- uspto-grants-2014_11
- 특허 번호
- US08889730B2
연결된 노트
불러오는 중…