Chloroacetaldehyde → HCID 90412925, 화합물
반응식
[NH2:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=[O:9])[C:5]([CH3:11])=[CH:4][CH:3]=1.[OH-].[Na+].Cl[CH2:15][CH:16]=O>O>[CH3:11][C:5]1[CH:4]=[CH:3][C:2]2[N:7]([CH:15]=[CH:16][N:1]=2)[C:6]=1[C:8]([OH:10])=[O:9]참가 물질
5
반응 조건
- 온도
- 150 °C
실험 절차
To the title compound of Step A (340 mg, 2.2 mmol) in H2O (7 mL) was added 1M aq. NaOH (2.2 mL, 2.2 mmol) and chloroacetaldehyde (210 μL, 3.4 mmol) and the reaction mixture heated in a microwave reactor at 150° C. for 2 h. Additional 1M aq. NaOH (2.2 mL, 2.2 mmol) and chloroacetaldehyde (210 μL, 3.4 mmol) were added and heating continued at 150° C. for 2 h. The reaction was purified via prep HPLC to give the title compound (282 mg, 72%). MS (ESI) mass calcd. for C9H8N2O2, 176.1; m/z found 177.0 [M+H]+.
후처리
- temperatureheating
- customThe reaction was purified via prep HPLC
출처 및 근거
- ORD 기록
- ord-70218fa18f3e41579a0c2898fc8eb921
- 출처 데이터셋
- uspto-grants-2015_06
- 특허 번호
- US09062078B2
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