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HCID 178433563, 화합물 → 4-(4-Methyl-1,3-thiazol-5-yl)benzonitrile

HRID 2107684
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HRID 2107684 반응식
[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]
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참가 물질

4

반응물 1

HCID 178433563HCID 178433563, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 935Nickel촉매2회HCID 702Ethanol용매

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온도
80 °C

실험 절차

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 a gum which solidified on standing (0.36 g, 35%), and was used directly in Preparation 19.

후처리

  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)

출처 및 근거

ORD 기록
ord-96a40f4ffcf1450c83568e4bd53e4c99
출처 데이터셋
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04935430

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