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Dimethylamine → HCID 12668361, 화합물

HRID 1973179
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인쇄 미리보기

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HRID 1973179 반응식
CNCCNCCNC.CNC.[CH3:13][N:14]([CH3:22])[P:15]([N:19]([CH3:21])[CH3:20])[N:16]([CH3:18])[CH3:17]>>[CH3:13][N:14]1[CH2:22][CH2:21][N:19]2[P:15]1[N:16]([CH3:18])[CH2:17][CH2:20]2
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참가 물질

4

반응물 3

HCID 674Dimethylamine2회HCID 15355Hexamethylphosphorous triamideHCID 3706439N,N'-(Iminobisethylene)bismethanamine

생성물 1

HCID 12668361HCID 12668361, 화합물수율 95%

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온도
125 °C

실험 절차

A mixture of 5.00 g of 1,7-dimethyldiethylenetriamine and 6.22 g of hexamethylphosphorous triamide is heated to 80° C, at which temperature dimethylamine begins to be evolved. Evolution of dimethylamine continues for about one hour, during which time the temperature is gradually raised to 125° C. The mixture is distilled to give 5.75 g (95%) of 2,8-dimethyl-2,5,8-triaza-1-phosphabicyclo[3.3.0]octane as a clear, colorless liquid, which boils at 55°-65° C at 0.30 mm. The nuclear magnetic-resonance spectrum (C6D6 /TMS) of the product shows a highly split pattern from δ 2.0 to 4.5 and has the expected sharp doublet for the --CH3 groups at δ 2.55, J = 10 Hz. The infrared absorption spectrum (neat) has absorptions at 3.5, 6.83, 6.91, 7.65, 7.80, 8.20, 8.68, 9.20, 9.70, 10.15, 10.4, 10.7, and 11.5 μ.

후처리

  1. distillationThe mixture is distilled

출처 및 근거

ORD 기록
ord-e14c8f900a3c47189fce595e95fcab9c
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03996276

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