Benzylamine → AC1Mdmfl

HRID 1780217노트

반응식

HRID 1780217 반응식
[Cl:1][CH2:2][P:3]([CH2:6]Cl)(=[O:5])[OH:4].[CH2:8]([NH2:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>>[ClH:1].[CH2:8]([NH:15][CH2:2][P:3]([CH2:6][NH:15][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:5])[OH:4])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

3

반응물 2

HCID 7504BenzylamineHCID 574694Bis(chloromethyl)phosphinic acid

생성물 1

HCID 2839277AC1Mdmfl

반응 조건

온도
115 °C

실험 절차

12 g (74 mmol) of bis(chloromethyl)phosphinic acid are added slowly to 80 g of benzylamine at room temperature while stirring, during which the temperature increases slightly. The mixture is then heated at 115° C. for 24 h. Excess benzylamine is removed by distillation in vacuo, and the white residue is dissolved in 150 ml of distilled water, filtered and mixed with 30 mi of concentrated HCl and stirred at room temperature for 1 h. The white precipitate is filtered off with suction, washed with water and dried over P2O5. Yield: 20 g (79%); m.p.: 254° C.

후처리

  1. temperatureincreases slightly
  2. customExcess benzylamine is removed by distillation in vacuo
  3. dissolutionthe white residue is dissolved in 150 ml of distilled water
  4. filtrationfiltered
  5. additionmixed with 30 mi of concentrated HCl
  6. stirringstirred at room temperature for 1 h
  7. filtrationThe white precipitate is filtered off with suction
  8. washwashed with water
  9. dry with materialdried over P2O5

출처 및 근거

ORD 기록
ord-7413cd76a3d14d178dc63224d0fe8ee5
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05629431

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