Oxalyl chloride → HCID 59627906、化合物
反応式
[CH3:1][C:2](=[CH2:10])[CH2:3][CH2:4][CH2:5][CH2:6][C:7](O)=[O:8].C(Cl)(=O)C([Cl:14])=O>C1C=CC=CC=1>[CH3:1][C:2](=[CH2:10])[CH2:3][CH2:4][CH2:5][CH2:6][C:7]([Cl:14])=[O:8]参加物
4
実験手順
To a solution of the carboxylic acid 71 (2.2 g, 15.5 mmol) in benzene (30 ml), was added oxalyl chloride (3 ml, 34.4 mmol, 2.22 equiv). A drying tube was placed on the flask and the reaction mixture was stirred for 90 min at room temperature before it was concentrated in vacuo. The crude acid chloride was used in the next step without further purification: TLC Rf=0.37 (silica gel, 25% EtOAc/hexanes); 1H NMR (600 MHz, CDCl3) δ 4.69 (s, 1H), 4.67 (s, 1H), 2.90-2.87 (t, 3J=7.8 Hz, 2H), 2.03-2.00 (t, 3J=7.8 Hz, 2H), 1.74-1.66 (m, 2H), 1.69 (s, 3H), 1.58-1.46 (m, 2H); 13C NMR (100 MHz, CDCl3) δ 173.979, 145.086, 110.717, 46.663, 37.334, 26.421, 24.799, 22.431.
後処理
- customA drying tube was placed on the flask
- concentrationwas concentrated in vacuo
- customThe crude acid chloride was used in the next step without further purification
出典と根拠
- ORDレコード
- ord-66e15831dc7b496d8ff6901b4fa8ffb5
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07893268B2
反応ノート
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