N,N'-Dimethylurea → Phosphonium, tetrakis((methyl((methylamino)carbonyl)amino)methyl)-,chloride

HRID 903530노트

반응식

HRID 903530 반응식
[CH2:1]([P+:3]([CH2:8]O)([CH2:6]O)[CH2:4]O)O.[Cl-:10].[CH3:11][NH:12][C:13]([NH:15][CH3:16])=[O:14]>>[Cl-:10].[CH3:11][N:12]([CH2:8][P+:3]([CH2:1][N:12]([CH3:11])[C:13]([NH:15][CH3:16])=[O:14])([CH2:4][N:12]([CH3:11])[C:13]([NH:15][CH3:16])=[O:14])[CH2:6][N:12]([CH3:11])[C:13]([NH:15][CH3:16])=[O:14])[C:13]([NH:15][CH3:16])=[O:14]

참가 물질

3

반응물 2

HCID 7293N,N'-DimethylureaHCID 31298Tetrakis(hydroxymethyl)phosphonium chloride

생성물 1

HCID 153314Phosphonium, tetrakis((methyl((methylamino)carbonyl)amino)methyl)-,chloride수율 25%

실험 절차

A solution of 80% THPC (59.55 g, 0.25 mol) and 1,3-dimethylurea (88.12 g, 1 mol) was heated to reflux in an oil bath, held at reflux for 4 hrs., allowed to cool, and stripped to dryness in a rotary evaporator. The residue (130.67 g) was shaken with acetonitrile (100 ml) and filtered, giving 29.40 g (25.0%) of tetrakis(1,3-dimethylureidomethyl)phosphonium chloride (I, R=R'=CH3, R"=H, X=Cl) as a white, crystalline solid, mp 189°-190° C. dec. The remainder, a heavy oil, yielded no more product nor water even when subjected to azeotropic distillation with toluene and more 1,3-dimethylurea.

후처리

  1. temperatureto reflux in an oil bath
  2. temperatureat reflux for 4 hrs
  3. temperatureto cool
  4. customstripped to dryness in a rotary evaporator
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-fad0fa7e9fd14f97b243c095cb17b139
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04228100

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