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HCID 178433563、化合物 → 4-(4-Methyl-1,3-thiazol-5-yl)benzonitrile

HRID 892778
ノート
印刷プレビュー

反応式

HRID 892778 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[S:13][C:12](S)=[N:11][C:10]=2[CH3:15])=[CH:5][CH:4]=1)#[N:2]>[Ni].C(O)C>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([C:9]2[S:13][CH:12]=[N:11][C:10]=2[CH3:15])=[CH:7][CH:8]=1)#[N:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 178433563HCID 178433563、化合物

生成物 1

HCID 198771814-(4-Methyl-1,3-thiazol-5-yl)benzonitrile

試薬・触媒・溶媒 2

HCID 935Nickel触媒2 回HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

Raney Nickel (1 g) was added to a solution of the product of (a) (1.2 g, 5 mmol) in absolute ethanol (120 ml) and the reactants heated at 80° C. in an autoclave for 18 hours. After cooling to ambient temperature, further Raney Nickel (1 g) was added to the reaction mixture and the reactants heated at 80° C. in an autoclave for an additional 6 hours. The reaction mixture was then filtered through Arbocel and the filtrate evaporated to dryness. The residue was flash chromatographed (Merck 60 Kieselgel--ethyl acetate:hexane:diethylamine, 25:75:2) to give the title product as a gum which solidified on standing (0.36 g, 35%), and was used directly in Preparation 19.

後処理

  1. temperatureAfter cooling to ambient temperature
  2. temperaturethe reactants heated at 80° C. in an autoclave for an additional 6 hours
  3. filtrationThe reaction mixture was then filtered through Arbocel
  4. customthe filtrate evaporated to dryness
  5. customchromatographed (Merck 60 Kieselgel--ethyl acetate:hexane:diethylamine, 25:75:2)

出典と根拠

ORDレコード
ord-2aee1b9952114c49a33416008755bbe8
出典データセット
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05120747

反応ノート

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