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2-Propanone, 1-(2-nitrophenoxy)- → 3-Methyl-3,4-dihydro-2H-1,4-benzoxazine

HRID 1515071
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반응식

HRID 1515071 반응식
[H][H].[N+:3]([C:6]1[CH:16]=[CH:15][CH:14]=[CH:13][C:7]=1[O:8][CH2:9][C:10](=O)[CH3:11])([O-])=O.[N+](C(OC1C=CC=CC=1)C(=O)C)([O-])=O>[Ni].CO>[CH3:11][CH:10]1[NH:3][C:6]2[CH:16]=[CH:15][CH:14]=[CH:13][C:7]=2[O:8][CH2:9]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 792392-Propanone, 1-(2-nitrophenoxy)-HCID 86645093Nitrophenoxyacetone2회HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 27637603-Methyl-3,4-dihydro-2H-1,4-benzoxazine

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

반응 조건

온도
40 °C

실험 절차

Reaction conditions: 220 bar of hydrogen, reaction temperature 60° C. with a residence time of about 60-90 minutes. The space velocity was about 2 g of o-nitrophenoxyacetone per g of catalyst used and hour. The catalyst used was a nickel sponge metal catalyst from H. C. Starck, Amperkat Ni—Mo 3706 (exchange of the water under which the catalyst is stored for methanol). The yields in this step were 95+%; at least 100 g of nitrophenoxyacetone were converted per gram of theoretically dry catalyst. Good mixing was ensured by stirring. In order to prevent precipitation of the reactant solution, it was heated to 40° C.

후처리

  1. customReaction conditions
  2. waitused and hour
  3. customThe yields in this step
  4. additionGood mixing
  5. customprecipitation of the reactant solution, it

출처 및 근거

ORD 기록
ord-629711ecd6cc4ed6aa253eec72c81650
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08222408B2

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