反応式
[C:1]([Cl:4])(Cl)=[O:2].[C:5]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15]O)=[CH:11][CH:10]=1)(=[O:7])[CH3:6]>C1(C)C=CC=CC=1>[C:5]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][C:1]([Cl:4])=[O:2])=[CH:11][CH:10]=1)(=[O:7])[CH3:6]参加物
4
実験手順
To a solution of phosgene in toluene (20% w/w, 2.2 mL, 4.2 mmol), cooled in an ice bath, was added dropwise a solution of 60 (321 mg, 1.9 mmol) in 2 mL of toluene. The mixture was stirred in the same bath, which was left to come to room temperature on its own. After 18 h, the mixture was concentrated in vacuo to give 61, which was used in the next step without further purification. 1H NMR (400 MHz, CDCl3) δ 2.30 (s, 3H), 5.28 (s, 2H), 7.13 (d, J=8.6 Hz, 2H), 7.42 (d, J=8.7 Hz, 2H).
後処理
- waitwas left
- customto come to room temperature on its
- concentrationthe mixture was concentrated in vacuo
出典と根拠
- ORDレコード
- ord-92490217d32c40b8aa54f432ecaf61a4
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524691B2
関連ノート
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