Hydrazine hydrate (1:1) → 6-(2-Methyl-1,3-dioxolan-2-yl)hexan-1-amine
반응식
[CH3:1][C:2]1([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][N:13]2C(=O)C3=CC=CC=C3C2=O)[O:6][CH2:5][CH2:4][O:3]1.O.NN>C(O)C>[CH3:1][C:2]1([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][NH2:13])[O:3][CH2:4][CH2:5][O:6]1참가 물질
4
실험 절차
A mixture of 125.25 g (0.395 mole) of N-[6-(2-methyl-1,3-dioxolan-2-yl)hexyl]phthalimide, 23 ml of 85% hydrazine hydrate, and 370 ml of 95% ethanol was refluxed for four hours, cooled, filtered and stripped. The residue was mixed with 500 ml of water, basified with 2 N NaOH solution and extracted with methylene chloride. The organic layer was separated, dried over anhydrous potassium carbonate, filtered, and stripped to an orange oil. This material was distilled to give 35.70 g (64%) of clear oil bp 80°-83° (0.100 mm).
후처리
- temperaturewas refluxed for four hours
- temperaturecooled
- filtrationfiltered
- additionThe residue was mixed with 500 ml of water
- extractionextracted with methylene chloride
- customThe organic layer was separated
- dry with materialdried over anhydrous potassium carbonate
- filtrationfiltered
- distillationThis material was distilled
출처 및 근거
- ORD 기록
- ord-82eb6438fb3043a6a2c519dfd2fb909c
- 출처 데이터셋
- uspto-grants-1983_01
- 특허 번호
- US04370335
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