Imidazole → 7-Chloro-4-methyl-4-trimethylsilyloxy-1-heptyne

HRID 126704노트

반응식

HRID 126704 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([OH:10])([CH3:9])[CH2:6][C:7]#[CH:8].CN(C)C=O.N1C=CN=C1.Cl[Si:22]([CH3:25])([CH3:24])[CH3:23]>O>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([CH3:9])([O:10][Si:22]([CH3:25])([CH3:24])[CH3:23])[CH2:6][C:7]#[CH:8]

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 6397ChlorotrimethylsilaneHCID 128987397-Chloro-4-hydroxy-4-methyl-1-heptyne

생성물 1

HCID 128987407-Chloro-4-methyl-4-trimethylsilyloxy-1-heptyne

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 7-chloro-4-hydroxy-4-methyl-1-heptyne in 80 ml. of dimethylformamide at 0° C., is added 43.8 g. (0.644 moles) of imidazole and 35.02 g. (0.322 moles of) chlorotrimethylsilane. The mixture is stirred at room temperature for 45 minutes, poured into water and extracted with hexane. The hexane solution is washed with dilute sodium bicarbonate solution, dried over magnesium sulfate and the solvent removed leaving an orange liquid. This liquid is distilled giving the desired product in the fraction boiling at 83°-88° C., 1.5 mm. as a colorless liquid.

후처리

  1. extractionextracted with hexane
  2. washThe hexane solution is washed with dilute sodium bicarbonate solution
  3. dry with materialdried over magnesium sulfate
  4. customthe solvent removed
  5. customleaving an orange liquid
  6. distillationThis liquid is distilled

출처 및 근거

ORD 기록
ord-d1e166c13c174a6c83e8b1a0087a4f0b
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254036

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