1-Chloroethyl chloroformate → 2-Chloro-5,6,7,8-tetrahydro-1,6-naphthyridine hydrochloride
반응식
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]=1참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-61d04bec5bf443a5be92d9634b722e5b
- 출처 데이터셋
- uspto-grants-2010_09
- 특허 번호
- US07795262B2
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