Chlorotrimethylsilane → HCID 23355510、化合物

HRID 234755ノート

反応式

HRID 234755 の反応式
[CH3:1][CH:2]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[C:4]([CH3:11])=[C:3]1[CH3:12].[H-].[K+].[H][H].[CH3:17][Si:18](Cl)([CH3:20])[CH3:19]>O>[CH3:1][CH:2]1[C:10]2[CH2:9][CH2:8][CH2:7][CH:6]([Si:18]([CH3:20])([CH3:19])[CH3:17])[C:5]=2[C:4]([CH3:11])=[C:3]1[CH3:12]

参加物

6

反応物 4

HCID 6397ChlorotrimethylsilaneHCID 82127Potassium hydride2 回HCID 186946261,2,3-Trimethyl-4,5,6,7-tetrahydro-1H-indeneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 23355510HCID 23355510、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

19.6 g of 1,2,3-trimethyl-4,5,6,7-tetrahydroindene as obtained in Example 1-(3) was dissolved in 70 mL of tetrahydrofuran anhydride. Then the resultant solution was added dropwise at room temperature to 200 mL of suspension of 7.2 g of potassium hydride in tetrahydrofuran anhydride. After the elapse of 1.5 hour, the mixed solution was gradually heated and the reaction was continued under refluxing with heating for 4 hours. When hydrogen was no longer generated, the reaction solution was restored to room temperature, incorporated with 19.6 g of trimethylsilyl chloride and stirred for two days and nights. Subsequently water was added to the reaction liquid to stabilize the excess potassium hydride, then the organic phase was separated, extraction was carried out from the water phase by the use of ethyl ether and the mixture of the extract and the aforesaid organic phase was dried with magnesium sulfate anhydride. Lastly, vacuum distillation was performed to recover 22.7 g of 1,2,3-trimethyl-4,5,6,7-tetrahydroindenyltrimethylsilane.

後処理

  1. temperatureAfter the elapse of 1.5 hour, the mixed solution was gradually heated
  2. temperatureunder refluxing
  3. temperaturewith heating for 4 hours
  4. customthe organic phase was separated
  5. extractionextraction
  6. additionthe mixture of the
  7. extractionextract
  8. dry with materialthe aforesaid organic phase was dried with magnesium sulfate anhydride
  9. distillationLastly, vacuum distillation
  10. customto recover 22.7 g of 1,2,3-trimethyl-4,5,6,7-tetrahydroindenyltrimethylsilane

出典と根拠

ORDレコード
ord-0c96d3cace50412fae1a3fb075bd51b3
出典データセット
uspto-grants-1997_01
特許番号
US05596054

反応ノート

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