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Water → HCID 178517472, 화합물

HRID 2389812
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HRID 2389812 반응식
[C:1]([CH:3]=[C:4]([NH:15]C(=O)OCC)[C:5]1[CH:10]=[CH:9][C:8]([C:11]([F:14])([F:13])[F:12])=[CH:7][CH:6]=1)#[N:2].[NH:21]([C:23](=[O:27])C(O)=O)[NH2:22].O.[C:29](OCC)(=O)C>CN1C(=O)CCC1>[F:12][C:11]([F:14])([F:13])[C:8]1[CH:9]=[CH:10][C:5]([C:4]2[N:15]=[C:23]([OH:27])[N:21]3[N:22]=[CH:29][N:2]=[C:1]3[CH:3]=2)=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 8857Ethyl AcetateHCID 222877Hydrazino(oxo)acetic acidHCID 76754610Ethyl {2-cyano-1-[4-(trifluoromethyl)phenyl]ethenyl}carbamate

생성물 1

HCID 178517472HCID 178517472, 화합물

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
160 °C

실험 절차

2.00 g (7.0 mmol) of ethyl [2-cyano-1-(4-trifluoromethylphenyl)ethenyl]carbamate (Example 129A) and 0.73 g (7.0 mmol) of hydrazino(oxo)acetic acid are dissolved in NMP (7 ml) under argon and stirred in a flask with a calcium chloride drying tube at an oil-bath temperature of 160° C. for 4 h. The reaction mixture is cooled to RT, mixed with water (20 ml) and stirred for 20 min. Ethyl acetate (150 ml) and water (100 ml) are added, and the organic phase is separated off, dried with magnesium sulphate and concentrated. The residue is suspended in water in an ultrasonic bath for 10 min. and then stirred for 30 min. The solid is filtered off and dried. 0.97 g (38% of theory) of the product are obtained.

후처리

  1. temperatureThe reaction mixture is cooled to RT
  2. stirringstirred for 20 min
  3. customthe organic phase is separated off
  4. dry with materialdried with magnesium sulphate
  5. concentrationconcentrated
  6. waitThe residue is suspended in water in an ultrasonic bath for 10 min.
  7. stirringstirred for 30 min
  8. filtrationThe solid is filtered off
  9. customdried
  10. custom0.97 g (38% of theory) of the product are obtained

출처 및 근거

ORD 기록
ord-ed95229fbbd6484baa71c8cee35fb1aa
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08273752B2

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