Hydrochloric Acid → HCID 178468827、化合物

HRID 620235ノート

反応式

HRID 620235 の反応式
[C:1]([CH2:3][C:4]1[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=1)#[N:2].C([Sn]([N:28]=[N+:29]=[N-:30])(CCCC)CCCC)CCC.Cl>COCCOC.CO>[NH:28]1[C:1]([CH2:3][C:4]2[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=2)=[N:2][N:30]=[N:29]1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 4984872Tributyltin azideHCID 11989373ethyl 4-(cyanomethyl)benzoate

生成物 1

HCID 178468827HCID 178468827、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
85 °C

実験手順

Ethyl 4-cyanomethylbenzoate (approximately 8 g) was dissolved in DME (10 ml). The solution was added tris(n-butyl)tin azide (5 ml) and the resultant solution was stirred and heated at 85° C. overnight. The solution was cooled to room temperature. The cooled solution was diluted with methanol then acidified with 1N hydrochloric acid. The acidified mixture was stirred for one hour then partitioned between ethyl acetate and water. The organic layer was separated, dried over magnesium sulfate, filtered, and concentrated in vacuo.

後処理

  1. temperatureThe solution was cooled to room temperature
  2. customthen partitioned between ethyl acetate and water
  3. customThe organic layer was separated
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7a561e537421461a8231b4ad5f12dbd9
出典データセット
uspto-grants-1989_04
特許番号
US04820723

反応ノート

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