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

HRID 848915노트

반응식

HRID 848915 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.CN(C)C=O.Cl[Si:27]([CH3:30])([CH3:29])[CH3:28]>CCCCCC>[CH3:28][Si:27]([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])([CH3:30])[CH3:29]

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 6397ChlorotrimethylsilaneHCID 127861934-Trimethylsilylethynyl-1-octyn-4-ol

생성물 1

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

시약·촉매·용매 1

HCID 8058Hexane용매

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. additionTo a stirred mixture of 8.5 g
  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
  7. customgiving 11.1 g

출처 및 근거

ORD 기록
ord-884fecd0d3004638add1de794f224d2b
출처 데이터셋
uspto-grants-1981_10
특허 번호
US04297516

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