Trimethylsilyl cyanide → HCID 86741182, 화합물

HRID 979800노트

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HRID 979800 반응식
[CH3:1][O:2][C:3]1[C:12]([O:13][CH3:14])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][CH2:7][C:8]2=O.[Cl-].[Al+3].[Cl-].[Cl-].C[Si]([C:24]#[N:25])(C)C>C1C=CC=CC=1>[C:24]([CH2:1][O:2][C:3]1[C:12]([O:13][CH3:14])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][CH:7]=[CH:8]2)#[N:25]

참가 물질

5

반응물 3

HCID 82115Trimethylsilyl cyanideHCID 6451240Aluminum(III) ChlorideHCID 82192465,6-dimethoxy-1-tetralone

생성물 1

HCID 86741182HCID 86741182, 화합물수율 96%

시약·촉매·용매 1

HCID 241Benzene용매

반응 조건

온도
70 °C

실험 절차

5,6-dimethoxytetralone (20 g) was dissolved in benzene (20 ml) and trimethylsilyl cyanide (16 ml). A catalytic amount of aluminum chloride was added and the reaction heated at 70° C. under nitrogen for 30 minutes. The volatiles were removed in vacuo and methanol (20 ml) added. Gaseous hydrochloric acid was bubbled through the methanol solution for 30 minutes resulting in precipitation of a solid. Stirring was continued for 1 hour, then the mixture was filtered and dried affording 19.9 g. of product (96% yield); m.p. 138°-9° C.

후처리

  1. customThe volatiles were removed in vacuo and methanol (20 ml)
  2. additionadded
  3. customGaseous hydrochloric acid was bubbled through the methanol solution for 30 minutes
  4. customresulting in precipitation of a solid
  5. filtrationthe mixture was filtered
  6. customdried
  7. customaffording 19.9 g

출처 및 근거

ORD 기록
ord-288484d9dbb34f1cbfe76439061ad0e6
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04634705

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