Oxalyl chloride → 2-Methyl-4,4,4-trifluorobutyryl chloride
반응식
[CH3:1][CH:2]([CH2:6][C:7]([F:10])([F:9])[F:8])[C:3](O)=[O:4].C(Cl)(=O)C([Cl:14])=O>C(Cl)Cl.CN(C)C=O>[CH3:1][CH:2]([CH2:6][C:7]([F:10])([F:9])[F:8])[C:3]([Cl:14])=[O:4]참가 물질
5
실험 절차
To 2-methyl-4,4,4-trifluorobutyric acid (172 g) in methylene chloride (150 mL) and N,N-dimethylformamide (3.5 mL) at 0° C., under nitrogen was added (dropwise) oxalyl chloride (125 mL). The mixture was allowed to warm to ambient temperature and stirred for 16 hours. After distillation of the solvent, distillation using a concentric tube distillation column (40 cm×15 mm) afforded 2-methyl-4,4,4-trifluorobutyryl chloride (about 99% purity, 79.87 g, 42%); bp 115.0°-116.0° C. (at atmospheric pressure, measured at room temperature as 763.27 mm Hg); GLC: tR =5.04 min; MS(CI): 139 (M+H-HCl).
후처리
- distillationAfter distillation of the solvent, distillation
- distillationdistillation column (40 cm×15 mm)
출처 및 근거
- ORD 기록
- ord-d206d4ce16cc4b8a804708e1a5b55863
- 출처 데이터셋
- uspto-grants-1994_08
- 특허 번호
- US05334765
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