Dimethylamine → Hexahydro-2a,5a,8a-triaza-8b-phospha-acenaphthylene

HRID 1973178

반응식

HRID 1973178 반응식
[NH:1]1[CH2:11][CH2:10][CH2:9][NH:8][CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.CNC.CN(C)[P:17](N(C)C)N(C)C>>[N:1]12[P:17]3[N:4]([CH2:5][CH2:6][CH2:7][N:8]3[CH2:9][CH2:10][CH2:11]1)[CH2:3][CH2:2]2

참가 물질

4

반응물 3

HCID 674DimethylamineHCID 15355Hexamethylphosphorous triamideHCID 3987421,4,8-Triazacycloundecane

생성물 1

HCID 23414755Hexahydro-2a,5a,8a-triaza-8b-phospha-acenaphthylene수율 75.2%

반응 조건

온도
125 °C

실험 절차

A mixture of 3.62 g of 1,4,8-triazacycloundecane and 3.75 g of hexamethylphosphorous triamide is heated to 125° C with stirring and held at this temperature for 2 hours, by which time evolution of dimethylamine is complete. Evolution is vigorous for the first 45 minutes. Distillation affords 3.20 g (75%) 1,4,8-triaza-12-phosphatricyclo-[6.3.1.04,12 ]dodecane as a water-white liquid which boils at 73°-75° C at 0.30 mm.

후처리

  1. customis vigorous for the first 45 minutes
  2. distillationDistillation

출처 및 근거

ORD 기록
ord-b13e99e974744e3a9603d095231b7332
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03996276

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