Methyl iodide → HCID 57936246、化合物

HRID 1434913ノート

反応式

HRID 1434913 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][CH2:7][CH2:8][CH2:9][OH:10].[H-].[Na+].I[CH3:14]>C1COCC1.O>[CH3:14][O:10][CH2:9][CH2:8][CH2:7][CH2:6][C:2]1[S:1][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 126238624-(Thiophen-2-yl)butan-1-ol

生成物 1

HCID 57936246HCID 57936246、化合物

試薬・触媒・溶媒 2

HCID 962Water触媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
50 °C

実験手順

A solution of 4-thiophen-2-yl-butan-1-ol (4.55 g, 29.09 mmol) in 20 ml of THF was carefully added to a stirred suspension of oil-free sodium hydride (1.05 g, 43.75 mmol) in 15 ml of THF. When the addition was complete, the mixture was heated to 50° C. and stirring continued for 1 hour. Iodomethane (2.7 ml, 43.75 mmol) was then added and the turbid solution was stirred at 50° C. for another 2 hours. After cooling, a few drops of water were added and the mixture was partitioned between 1N-HCl and ether. The organic layer was washed with saturated sodium bicarbonate solution and brine. Drying over sodium sulfate and careful evaporation (product is volatile) gave a pale yellow oil. Yield: 4.45 g (90%).

後処理

  1. additionWhen the addition
  2. stirringthe turbid solution was stirred at 50° C. for another 2 hours
  3. temperatureAfter cooling
  4. customthe mixture was partitioned between 1N-HCl and ether
  5. washThe organic layer was washed with saturated sodium bicarbonate solution and brine
  6. dry with materialDrying over sodium sulfate and careful evaporation (product is volatile)
  7. customgave a pale yellow oil

出典と根拠

ORDレコード
ord-eb1b806ff2da40a4b56a946a1ca4317a
出典データセット
uspto-grants-2009_11
特許番号
US07615562B2

反応ノート

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