Methyl iodide → HCID 57936246, 화합물

HRID 1434913노트

반응식

HRID 1434913 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 57936246HCID 57936246, 화합물

시약·촉매·용매 2

HCID 962Water촉매HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
50 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-eb1b806ff2da40a4b56a946a1ca4317a
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07615562B2

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