Water → 3-Methyl-3,4-dihydro-2H-1,4-benzoxazine

HRID 1515072

반응식

HRID 1515072 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.O.[N+](C(OC1C=CC=CC=1)C(=O)C)([O-])=O>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 물질

6

반응물 4

HCID 962WaterHCID 792392-Propanone, 1-(2-nitrophenoxy)-HCID 86645093NitrophenoxyacetoneHCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
40 °C

실험 절차

Reaction conditions: 150 bar of hydrogen, reaction temperature 80° 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 sponge metal catalyst from H. C. Starck, Amperkat Ni—Mo 3706 (exchange of the water under which the catalyst is stored for methanol). The yield was 90%; 42 g of nitrophenoxyacetone were converted per gram of theoretically dry catalyst. Thereafter, the hydrogenation had to be stopped owing to the massive formation of secondary components (in particular of the 3MBM dimer). 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. additionGood mixing
  4. customprecipitation of the reactant solution, it

출처 및 근거

ORD 기록
ord-54d56c0d9b33462987f5a633cd8612e1
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08222408B2

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