Dimethylformamide → HCID 54273058、化合物
反応式
[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]参加物
5
実験手順
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).
後処理
- custom(2 h)
- customthe solvent was evaporated under reduced pressure
- distillationthe residual liquid was distilled off (bulb to bulb) under vacuum
出典と根拠
- ORDレコード
- ord-0018c18d341e4d789be33a445f7b5141
- 出典データセット
- uspto-grants-1983_03
- 特許番号
- US04378314
反応ノート
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