반응식
[N+:1]([O-:4])([OH:3])=[O:2].C(OC(=O)C)(=O)C.O[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([Cl:20])[N:15]=1.C(=O)([O-])[O-].[K+].[K+]>>[O:2]([CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([Cl:20])[N:15]=1)[N+:1]([O-:4])=[O:3]참가 물질
5
실험 절차
Fuming nitric acid (1.57 ml) was added dropwise to acetic anhydride (3.54 ml) with stirring at 0° to 5° C. 2-Hydroxymethyl-6-chloropyridine (3.59 g) was added thereto. The resulting mixture was stirred for 20 minutes at 0° C. to 5° C. The resulting mixture was alkalized weakly with an aqueous potassium carbonate solution, extracted with chloroform, washed with water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue obtained was subjected to column chromatography on aluminum oxide (40 g) and eluted with toluene. The fractions containing the desired compound were concentrated under reduced pressure to give colorless viscous oil of 2-nitroxymethyl-6-chloropyridine (2.9 g).
후처리
- stirringThe resulting mixture was stirred for 20 minutes at 0° C. to 5° C
- extractionextracted with chloroform
- washwashed with water
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue obtained
- washeluted with toluene
- additionThe fractions containing the desired compound
- concentrationwere concentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-f535e02077c44014b2bb4eb7229d20aa
- 출처 데이터셋
- uspto-grants-1988_06
- 특허 번호
- US04749574
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