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Water → HCID 178517472、化合物

HRID 2389812
ノート
印刷プレビュー

反応式

HRID 2389812 の反応式
[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
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

6

反応物 4

HCID 962Water2 回HCID 8857Ethyl AcetateHCID 222877Hydrazino(oxo)acetic acidHCID 76754610Ethyl {2-cyano-1-[4-(trifluoromethyl)phenyl]ethenyl}carbamate

生成物 1

HCID 178517472HCID 178517472、化合物

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
160 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ed95229fbbd6484baa71c8cee35fb1aa
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08273752B2

反応ノート

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