Phenylphosphonic dichloride → HCID 22748773、化合物

HRID 1390329

反応式

HRID 1390329 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:9]2[CH:10]=[CH:11][C:12](=O)[NH:13][CH:14]=2)=[CH:4][CH:3]=1.C1(P(Cl)([Cl:30])=O)C=CC=CC=1>>[Cl:30][C:12]1[CH:11]=[CH:10][C:9]([CH:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:14][N:13]=1

参加物

3

実験手順

Combine 50 g. (0.174 mole) of the 5-substituted 2-pyridone from step A with 125 ml. of phenylphosphonic dichloride and heat at 210°-220° C. for about 7 hours with stirring. Allow to stand overnight and pour onto ice. Basify with ammonium hydroxide and extract with ethyl ether. Dry the ether solution and concentrate to a residue. Distill the residue and collect the fraction boiling at 205°-215° C. at 0.55 mm. (49 g.).

後処理

  1. additionpour onto ice
  2. extractionBasify with ammonium hydroxide and extract with ethyl ether
  3. dry with materialDry the ether solution
  4. concentrationconcentrate to a residue
  5. distillationDistill the residue
  6. customcollect the fraction boiling at 205°-215° C. at 0.55 mm

出典と根拠

ORDレコード
ord-db9f39e8ab614a5c9ef4e5f6d14a94c0
出典データセット
uspto-grants-1979_02
特許番号
US04138488

関連ノート

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