反応式
[OH:1][CH2:2][CH2:3][CH2:4][C:5](=O)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([OH:18])=[O:17].[OH-].[K+].C(O)COCCO.Cl>O>[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([OH:18])=[O:17]参加物
実験手順
1.00 g (3.68 millimole) of 15-hydroxy-12-ketopentadecanoic acid, 0.73 g (11.0 millimole) of 85 wt.% potassium hydroxide, 0.50 g (8.5 millimole) of 85 % hydrated hydrazine and 5 ml of diethylene glycol were charged into a frask and heated under reflux over 1.5 hours. Subsequently, while evaporating the produced light boiling components such as water to the outside of the system, the internal temperature was elevated to 195 to 205° C., and the heating under reflux was continued at the same temperature range over 2 hours. After completion of the reaction, the solution was cooled, diluted by addition of 5 ml of water and added with 3 ml of 6N-HCl, followed by collection of the precipitated pail brown solid by filtration. The solid was recrystallized from benzene to obtain 0.81 g (3.14 millimole, Yield: 85 %) of a white crystl.
後処理
- temperatureheated
- temperatureunder reflux over 1.5 hours
- customSubsequently, while evaporating the produced light
- customwas elevated to 195 to 205° C.
- temperaturethe heating under reflux
- customAfter completion of the reaction
- temperaturethe solution was cooled
- filtrationfollowed by collection of the precipitated pail brown solid by filtration
- customThe solid was recrystallized from benzene
- customto obtain 0.81 g (3.14 millimole, Yield: 85 %) of a white crystl
出典と根拠
- ORDレコード
- ord-bc798a77a48a49ffaf13ef4043394149
- 出典データセット
- uspto-grants-1991_06
- 特許番号
- US05023351
関連ノート
読み込み中…