反応式
[SH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13].[CH3:15]I.O=O.[OH-].[Na+]>O.C(O)C>[CH3:15][S:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13]参加物
実験手順
Into a 3-neck round-bottom flask fitted with a condenser and an addition funnel were added 20 g of 11-mercaptoundecanoic acid, 13 g of methyl iodide and 200 mL of ethanol. A slow flow of nitrogen through the reactor was started to exclude oxygen because mercaptans can be converted into disulfides in the presence of air and strong alkali. A solution of 7.33 g of sodium hydroxide in 14.66 g of water was added dropwise to the reaction mixture via the addition funnel. Any unreacted methyl iodide, the ethanol and the water were removed using a rotovap. The residue was acidified using a mixture of concentrated hydrochloric acid and ice. After isolation the product was distilled. After a small amount of a low boiling fraction was collected, the crude product was collected at ~1 mm of Hg at 180° C. weighing 22.75 g. The crude product was distilled to yield 12.5 g of desired product representing 58.7% of theoretical based upon the weight of starting 11-mercaptoundecanoic acid.
後処理
- customInto a 3-neck round-bottom flask fitted with a condenser and an addition funnel
- customAny unreacted methyl iodide, the ethanol and the water were removed
- additiona mixture of concentrated hydrochloric acid and ice
- distillationAfter isolation the product was distilled
- customAfter a small amount of a low boiling fraction was collected
- customthe crude product was collected at ~1 mm of Hg at 180° C.
- distillationThe crude product was distilled
出典と根拠
- ORDレコード
- ord-e056294faf58454b8bb2558941a3754a
- 出典データセット
- uspto-grants-1991_04
- 特許番号
- US05004558
関連ノート
読み込み中…