Imidazole → 1-Iodo-3-methyl-3-trimethylsilyloxy-1-octene

HRID 261384

反応式

HRID 261384 の反応式
[OH:1][C:2]([CH3:11])([CH2:6][CH2:7][CH2:8][CH2:9][CH3:10])[CH:3]=[CH:4][I:5].N1C=CN=C1.[CH3:17][Si:18](Cl)([CH3:20])[CH3:19].CCCCCC>CN(C)C=O>[I:5][CH:4]=[CH:3][C:2]([CH3:11])([O:1][Si:18]([CH3:20])([CH3:19])[CH3:17])[CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]

参加物

6

反応条件

温度
0 °C

実験手順

To a stirred solution of 11.7 g of 3-hydroxy-1-iodo-3-methyl-1-octene (Example 184) and 7.4 g of imidazole in 45 ml of dry dimethylformamide is added dropwise 5.98 g of trimethylsilylchloride at 0° C. under argon atmosphere. After stirring at 0° C. for an additional 15 minutes, the solution is stirred at ambient temperature for 18 hours. The reaction mixture is poured into 600 ml of hexane and the resulting solution washed with water, saturated sodium chloride solution, dried over anhydrous magnesium sulfate and taken to dryness to furnish 14.7 g of oil. Distillation affords 13.4 g of clear oil; bp 65° C. (0.05 mm); λ max 6.21, 8.00, 9.90, 10.51, 11.90, 13.2μ.

後処理

  1. stirringthe solution is stirred at ambient temperature for 18 hours
  2. washthe resulting solution washed with water, saturated sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate

出典と根拠

ORDレコード
ord-8daa7a0e283248c39835f9b53925402b
出典データセット
uspto-grants-1979_08
特許番号
US04165331

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