Trimethylsilyl cyanide → HCID 86741182、化合物

HRID 979800ノート

反応式

HRID 979800 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 86741182HCID 86741182、化合物収率 96%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-288484d9dbb34f1cbfe76439061ad0e6
出典データセット
uspto-grants-1987_01
特許番号
US04634705

反応ノート

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