Methyl iodide → HCID 178501284、化合物
反応式
[OH:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([C:8]([OH:10])=[O:9])[CH2:4][CH2:3]1.[C:11]([O-])([O-])=O.[K+].[K+].IC>CN(C=O)C.CCOC(C)=O>[CH3:11][O:9][C:8]([C@H:5]1[CH2:6][CH2:7][C@@H:2]([OH:1])[CH2:3][CH2:4]1)=[O:10]参加物
6
実験手順
To a solution of trans-4-hydroxycyclohexanecarboxylic acid (5.0 mmol, 721 mg), K2CO3 (15.0 mmol, 2.07 g) in DMF (17 mL) is added iodomethane (6.0 mmol, 0.374 mL). After stirring for 2 h, the mixture is diluted with EtOAc. The mixture is washed with H2O and brine, dried over Na2SO4 and concentrated. The residue is used to next reaction without further purification (643 mg, 81%); ESI-MS m/z: 159 [M+1]+, Retention time 1.34 min. (condition A).
後処理
- washThe mixture is washed with H2O and brine
- dry with materialdried over Na2SO4
- concentrationconcentrated
- customThe residue is used to next reaction without further purification (643 mg, 81%)
出典と根拠
- ORDレコード
- ord-d80ff8c0710145e385dfecaf90ac252b
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08193349B2
反応ノート
読み込み中…