Diphenyl Ether → HCID 22397178、化合物

HRID 1070641ノート

反応式

HRID 1070641 の反応式
[Cl:1][C:2]1[C:7]([NH:8][CH:9]=[C:10]([C:16]([O:18]CC)=O)[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:6][CH:5]=[C:4]([CH3:21])[N:3]=1.C1(OC2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[Cl:1][C:2]1[N:3]=[C:4]([CH3:21])[CH:5]=[C:6]2[C:7]=1[NH:8][CH:9]=[C:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:16]2=[O:18]

参加物

4

反応物 2

HCID 7583Diphenyl EtherHCID 22397139HCID 22397139、化合物

生成物 1

HCID 22397178HCID 22397178、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of diethyl 2-(((2-chloro-6-methyl-3-pyridinyl)amino)methylene)malonate (Preparation 42, 0.59 g) is added to diphenyl ether (15 mL) and the mixture is degassed by alternately bubbling in nitrogen then subjecting to high vacuum. The mixture is heated rapidly to reflux and after 30 minutes cooled to room temperature. Diphenyl ether is distilled away under high vacuum and the residue taken up in CH2Cl2 (40 mL). The solid is collected by filtration and washed with CH2Cl2 with a second crop obtained by reducing the solvent volume of CH2Cl2 filtrate and collecting more solid. The title compound is obtained as a pale green powder, 0.24 g (47%). Physical characteristics: MS (ESI+) m/z 267 (M+H).

後処理

  1. customthe mixture is degassed
  2. customby alternately bubbling in nitrogen
  3. temperatureThe mixture is heated rapidly
  4. temperatureto reflux and after 30 minutes
  5. distillationDiphenyl ether is distilled away under high vacuum
  6. filtrationThe solid is collected by filtration
  7. washwashed with CH2Cl2 with a second crop
  8. customobtained
  9. customcollecting more solid

出典と根拠

ORDレコード
ord-df177cf5d4d44f2b9178132efe9fd5c1
出典データセット
uspto-grants-2005_06
特許番号
US06903097B2

反応ノート

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