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Methanamine, 1-(dimethylphosphinyl)- → HCID 70461647、化合物

HRID 364608
ノート
印刷プレビュー

反応式

HRID 364608 の反応式
[F:1][C:2]([F:23])([F:22])[C:3]1[CH:4]=[CH:5][C:6]([O:9][C:10]2[CH:15]=[CH:14][C:13]([N+:16]([O-:18])=[O:17])=[C:12]([N+:19]([O-])=O)[CH:11]=2)=[N:7][CH:8]=1.[CH3:24][P:25](=[O:29])([CH2:27]N)[CH3:26]>C1(C)C=CC=CC=1>[N+:16]([C:13]1[CH:14]=[CH:15][C:10]([O:9][C:6]2[CH:5]=[CH:4][C:3]([C:2]([F:23])([F:22])[F:1])=[CH:8][N:7]=2)=[CH:11][C:12]=1[NH:19][CH2:24][P:25](=[O:29])([CH3:27])[CH3:26])([O-:18])=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 164269Methanamine, 1-(dimethylphosphinyl)-HCID 202299032-(3,4-Dinitrophenoxy)-5-(trifluoromethyl)pyridine

生成物 1

HCID 70461647HCID 70461647、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 4.97 g of (5-trifluoromethyl-2-pyridyloxy)-3,4-dinitrobenzene in 15 ml of toluene is refluxed, and 3.21 g of melted P,P-dimethyl-aminomethylphosphine oxide are added dropwise. The mixture is refluxed for a further 2 hours, nitrous gases being evolved at the start. The brown solution is subsequently concentrated by evaporation, and the residue is recrystallised from 50 ml of ethyl acetate to thus obtain 4.10 g (70% of theory) of N-[2-nitro-5-(5-trifluoromethyl-2-pyridyloxy)-phenyl]-P,P-dimethyl-aminomethylphosphine oxide in the form of yellow crystals, m.p. 158°-160° C.

後処理

  1. temperatureThe mixture is refluxed for a further 2 hours
  2. concentrationThe brown solution is subsequently concentrated by evaporation
  3. customthe residue is recrystallised from 50 ml of ethyl acetate to thus obtain 4.10 g (70% of theory) of N-[2-nitro-5-(5-trifluoromethyl-2-pyridyloxy)-phenyl]-P,P-dimethyl-aminomethylphosphine oxide in the form of yellow crystals, m.p. 158°-160° C.

出典と根拠

ORDレコード
ord-33f22be55f1f4313983cd6123b5ad69c
出典データセット
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04605434

反応ノート

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