Dimethylamine → Hexahydro-1H,4H,7H-3a,6a,9a-triaza-9b-phosphaphenalene

HRID 1973177

반응식

[NH:1]1[CH2:12][CH2:11][CH2:10][NH:9][CH2:8][CH2:7][CH2:6][NH:5][CH2:4][CH2:3][CH2:2]1.CNC.CN(C)[P:18](N(C)C)N(C)C>>[N:1]12[P:18]3[N:9]([CH2:8][CH2:7][CH2:6][N:5]3[CH2:4][CH2:3][CH2:2]1)[CH2:10][CH2:11][CH2:12]2

참가 물질

반응물 3

HCID 674Dimethylamine

HCID 15355Hexamethylphosphorous triamide

HCID 4707781,5,9-Triazacyclododecane

생성물 1

HCID 333382Hexahydro-1H,4H,7H-3a,6a,9a-triaza-9b-phosphaphenalene수율 76%

실험 절차

A mixture of 4.20 g of 1,5,9-triazacyclododecane and 4.00 g of hexamethylphosphorous triamide is heated at 100° C for about six hours, by which time evolution of dimethylamine is complete. Distillation under reduced pressure gives 3.70 g (76%) of 1,5,9-triaza-13-phosphatricyclo-[7.3.1.05,13 ]tridecane as a clear, colorless liquid which boils at 104°-135° C at 0.60 mm. The product solidifies at room temperature. Its infrared absorption spectrum (neat) shows absorptions at 3.5, 6.85, 7.01, 7.52, 7.73, 8.00, 8.27, 8.66, 8.90, 9.02, 9.36, 9.56, 10.27, 10.89, 11.42, 11.73, 11.97 and 14.7 μ. The mass spectrum shows an M+ ion at 199; measured mass, 199.1264; calc'd, 199.1238.

후처리

distillationDistillation under reduced pressure

출처 및 근거

ORD 기록: ord-ea1c9badf517452ebff33d295102bd0d
출처 데이터셋: uspto-grants-1976_12
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US03996276

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