Chlorotrimethylsilane → HCID 23355510, 화합물

HRID 234755노트

반응식

HRID 234755 반응식
[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]

참가 물질

6

반응물 4

HCID 6397ChlorotrimethylsilaneHCID 82127Potassium hydride2회HCID 186946261,2,3-Trimethyl-4,5,6,7-tetrahydro-1H-indeneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 23355510HCID 23355510, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0c96d3cace50412fae1a3fb075bd51b3
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05596054

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