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

HRID 225079

反応式

HRID 225079 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-1332913e923c4111b16b38886940cfdc
出典データセット
uspto-grants-1980_11
特許番号
US04235797

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