Dimethylformamide → HCID 54273058, 화합물
반응식
[N:1]([CH:4]([CH2:8][CH2:9][CH3:10])[C:5](O)=[O:6])=[N+:2]=[N-:3].C(Cl)(=O)C([Cl:14])=O.CN(C)C=O>ClCCl>[N:1]([CH:4]([CH2:8][CH2:9][CH3:10])[C:5]([Cl:14])=[O:6])=[N+:2]=[N-:3]참가 물질
5
실험 절차
A solution of (2R and 2S) 2-azidopentanoic acid (2.213 g, 15.46 mmol) in dry dichloromethane (20 ml) was treated with oxalyl chloride (1.57 ml, 18.55 mmol) and a drop of N,N-dimethyl formamide. After the evolution of gas had ceased (2 h), the solvent was evaporated under reduced pressure and the residual liquid was distilled off (bulb to bulb) under vacuum to give 2.224 g (89%) of a clear oil: bp 50°-55° C./5 torr (air bath temperature); ir (film) νmax : 2105 (N3), 1785 cm-1 (C=O); 1Hmr (CDCl3) δ: 4.1 (1H, dd, J=7, J=6, H-2), 2.2-1.2 (4H, m, H-3 and H-4), and 0.98 ppm (3H, distorted t, J=6, H-5).
후처리
- custom(2 h)
- customthe solvent was evaporated under reduced pressure
- distillationthe residual liquid was distilled off (bulb to bulb) under vacuum
출처 및 근거
- ORD 기록
- ord-853966cf179749c3ac17e97dc36206ab
- 출처 데이터셋
- uspto-grants-1981_06
- 특허 번호
- US04272437
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