Imidazole → 4-Methyl-4-trimethylsilyloxy-7-oxa-1octyne

HRID 126720

反応式

HRID 126720 の反応式
[OH:1][C:2]([CH3:10])([CH2:6][CH2:7][O:8][CH3:9])[CH2:3][C:4]#[CH:5].N1C=CN=C1.CN(C)C=O.[CH3:21][Si:22]([CH3:25])([CH3:24])Cl>CCCCCC>[CH3:10][C:2]([O:1][Si:22]([CH3:25])([CH3:24])[CH3:21])([CH2:6][CH2:7][O:8][CH3:9])[CH2:3][C:4]#[CH:5]

参加物

6

反応物 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 6397ChlorotrimethylsilaneHCID 127862294-Hydroxy-4-methyl-7-oxa-1-octyne

生成物 1

HCID 127862304-Methyl-4-trimethylsilyloxy-7-oxa-1octyne

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

To a solution of 13 g. (0.091 moles) of 4-hydroxy-4-methyl-7-oxa-1-octyne and 16 g. (0.235 moles) of imidazole in 80 ml. of dry dimethylformamide is added dropwise, at 5° C. under nitrogen with stirring, 12.5 ml. (0.115 moles) of trimethylchlorosilane. After an additional 15 minutes at 5° C. the solution is stirred at ambient temperature for 18 hours then added to 450 ml. of hexane. The resulting solution is washed with ice-cold water, ice-cold saturated sodium chloride solution, dried with anhydrous magnesium sulfate and taken to dryness in vacuo. Distillation of the residual oil furnishes 16.8 g. (86%) of product; b.p. 87°-88° C. (7 mm.).

後処理

  1. stirringAfter an additional 15 minutes at 5° C. the solution is stirred at ambient temperature for 18 hours
  2. additionthen added to 450 ml
  3. washThe resulting solution is washed with ice-cold water, ice-cold saturated sodium chloride solution
  4. dry with materialdried with anhydrous magnesium sulfate
  5. distillationDistillation of the residual oil
  6. customfurnishes 16.8 g

出典と根拠

ORDレコード
ord-f34628579d95474195ffc1b6186e5dbf
出典データセット
uspto-grants-1981_03
特許番号
US04254036

関連ノート

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