1-Chloroethyl chloroformate → 2-Chloro-5,6,7,8-tetrahydro-1,6-naphthyridine hydrochloride
反応式
C([N:8]1[CH2:17][CH2:16][C:15]2[N:14]=[C:13]([Cl:18])[CH:12]=[CH:11][C:10]=2[CH2:9]1)C1C=CC=CC=1.ClC(OC(Cl)C)=O>C(Cl)CCl>[ClH:18].[Cl:18][C:13]1[CH:12]=[CH:11][C:10]2[CH2:9][NH:8][CH2:17][CH2:16][C:15]=2[N:14]=1参加物
4
実験手順
A mixture of 6-benzyl-2-chloro-5,6,7,8-tetrahydro-1,6-naphthyridine (98 mg, 0.38 mmol) and 1-chloroethyl chloroformate (0.05 mL, 0.46 mmol) in ClCH2CH2Cl (10 mL) is refluxed for 3 hr. The solvent is removed and the residue is dissolved in MeOH (10 mL) and the mixture is reflux for 30 min. Solvent is removed in vacuo and the residue is stirred with ether (10 mL) for 30 min at rt and filtered. The resulting light brown solid is used in the next step without further purification. MS (M+1): 169.1.
後処理
- temperatureis refluxed for 3 hr
- customThe solvent is removed
- dissolutionthe residue is dissolved in MeOH (10 mL)
- temperaturethe mixture is reflux for 30 min
- customSolvent is removed in vacuo
- filtrationfiltered
- customThe resulting light brown solid is used in the next step without further purification
出典と根拠
- ORDレコード
- ord-61d04bec5bf443a5be92d9634b722e5b
- 出典データセット
- uspto-grants-2010_09
- 特許番号
- US07795262B2
反応ノート
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