反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][C:9](=[O:15])[C:10]2([CH3:14])[CH3:13])=[CH:5][CH:4]=1.[Cl:16][S:17](O)(=[O:19])=[O:18].C(Cl)(=O)C(Cl)=O.CN(C)C=O>ClCCl>[CH3:1][O:2][C:3]1[C:4]([S:17]([Cl:16])(=[O:19])=[O:18])=[CH:5][C:6]2[CH2:7][CH2:8][C:9](=[O:15])[C:10]([CH3:13])([CH3:14])[C:11]=2[CH:12]=1参加物
6
実験手順
To the dichloromethane (2 ml) solution of 7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound A2, 200 mg, 0.980 mmol), chlorosulfonic acid (110 μl, 1.70 eq.) was added and the mixture was stirred at room temperature for 2 hr. To the reaction solution, oxalyl chloride (297 μl, 3.0 eq.) and N,N-dimethyl formamide (45 μl, 0.6 eq.) were added in three divided portions, and the mixture was stirred at room temperature for 30 min. The reaction solution was concentrated under reduced pressure to obtain the title compound (295 mg). Since the title compound is unstable, its structure was identified in the next step.
後処理
- stirringthe mixture was stirred at room temperature for 30 min
- concentrationThe reaction solution was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-2fa1ffd1e766470883a444cac93df6c0
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09440922B2
関連ノート
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