Imidazole → 4-Trimethylsilylethynyl-1-octyn-4-ol trimethylsilyl ether

HRID 127083노트

반응식

HRID 127083 반응식
[CH3:1][Si:2]([C:5]#[C:6][C:7]([OH:15])([CH2:11][CH2:12][CH2:13][CH3:14])[CH2:8][C:9]#[CH:10])([CH3:4])[CH3:3].N1C=CN=C1.Cl[Si:22]([CH3:25])([CH3:24])[CH3:23].CCCCCC>CN(C)C=O>[CH3:23][Si:22]([O:15][C:7]([C:6]#[C:5][Si:2]([CH3:3])([CH3:1])[CH3:4])([CH2:11][CH2:12][CH2:13][CH3:14])[CH2:8][C:9]#[CH:10])([CH3:25])[CH3:24]

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 6397ChlorotrimethylsilaneHCID 8058HexaneHCID 127861934-Trimethylsilylethynyl-1-octyn-4-ol

생성물 1

HCID 572330774-Trimethylsilylethynyl-1-octyn-4-ol trimethylsilyl ether

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred mixture of 8.5 g of 4-trimethylsilylethynyl-1-octyn-4-ol and 6.2 g of imidazole in 24 ml of dry dimethylformamide is added, under nitrogen, 5.7 ml of chlorotrimethylsilane, in a slow stream, via a syringe. The mixture is stirred in an ice bath for one hour and then at room temperature overnight. The mixture is poured into hexane, washed with saturated sodium bicarbonate solution, water and then brine and dried over sodium sulfate. The solvents are evaporated to dryness giving 11.1 g of the desired product.

후처리

  1. additionis added, under nitrogen
  2. customat room temperature
  3. customovernight
  4. washwashed with saturated sodium bicarbonate solution, water
  5. dry with materialbrine and dried over sodium sulfate
  6. customThe solvents are evaporated to dryness

출처 및 근거

ORD 기록
ord-848e283b62bc4e9dbe467a8b2f0ef784
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254285

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