Potassium Hydroxide → 3-[(Dibenzylamino)oxy]propanoic acid
反応式
[CH2:1]([N:8]([CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[O:9][CH2:10][CH2:11][C:12]([O:14]C)=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[K+]>O1CCCC1.O>[CH2:16]([N:8]([CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[O:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13])[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1参加物
5
実験手順
A solution of 22.4 g of methyl 3-[N,N-dibenzylaminoxy]propanoate and 4.50 g of potassium hydroxide in 200 ml of tetrahydrofuran and 200 ml of water is heated under reflux for 12 hours under N2. The mixture is concentrated under reduced pressure and the residue is partitioned between water and ether. The combined aqueous extracts are acidified with hydrochloric acid and then extracted with methylene chloride. The combined organic extracts are dried (MgSO4) and evaporated under reduced pressure to afford the title compound as a pale yellow oil.
後処理
- temperatureunder reflux for 12 hours under N2
- concentrationThe mixture is concentrated under reduced pressure
- customthe residue is partitioned between water and ether
- extractionextracted with methylene chloride
- dry with materialThe combined organic extracts are dried (MgSO4)
- customevaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-c4040b9dd1044af0b6ee41a257c75a4d
- 出典データセット
- uspto-grants-1987_05
- 特許番号
- US04666962
反応ノート
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