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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 178517485、化合物

HRID 2171546
ノート
印刷プレビュー

反応式

HRID 2171546 の反応式
[C:1]([CH:3]=[C:4]([NH:13]C(=O)OCC)[C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:6]=1[Cl:12])#[N:2].[NH:19]([C:21](=[O:25])C(O)=O)[NH2:20].O.[C:27](OCC)(=O)C>CN1C(=O)CCC1>[Cl:12][C:6]1[CH:7]=[C:8]([Cl:11])[CH:9]=[CH:10][C:5]=1[C:4]1[N:13]=[C:21]([OH:25])[N:19]2[N:20]=[CH:27][N:2]=[C:1]2[CH:3]=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 76754608Ethyl[2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate

生成物 1

HCID 178517485HCID 178517485、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

500 mg (1.75 mmol) of ethyl [2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate (Example 128A) and 182 mg (1.75 mmol) of hydrazino(oxo)acetic acid are dissolved in NMP (2 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 stirred with diethyl ether/dichloromethane, and the solid is filtered off and dried. 150 mg (31% 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. stirringThe residue is stirred with diethyl ether/dichloromethane
  7. filtrationthe solid is filtered off
  8. customdried
  9. custom150 mg (31% of theory) of the product are obtained

出典と根拠

ORDレコード
ord-679120a205f349669541afcac107ac6d
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09051323B2

反応ノート

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