Hexamethylphosphorous triamide → HCID 23414757, compound

HRID 259490Notes

Reaction equation

[NH:1]1[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9][CH2:8][NH:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.CN(C)[P:17](N(C)C)N(C)C>>[N:1]12[P:17]3[N:11]([CH2:10][CH2:9][CH2:8][N:7]3[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1)[CH2:12][CH2:13][CH2:14]2

Participants

Reactant 2

HCID 15355Hexamethylphosphorous triamide

HCID 6397479HCID 6397479, compound

Product 1

HCID 23414757HCID 23414757, compound

Procedure

A stirred mixture of 6.00 g (30 mmol) of 1,4,7,11-tetraazacyclotetradecane and 4.90 g of hexamethylphosphorous triamide is heated under nitrogen for 3 hr at 120° and then distilled in a short-path apparatus to give 5.50 g (80%) of clear, colorless liquid 1,5,9,12-tetraaza-15-phosphatricyclo[7.5.1.05,15 ]pentadecane, bp 106°-110° (0.30 mm), which solidifies on storing below 0°.

Workup

temperatureis heated under nitrogen for 3 hr at 120°
distillationdistilled in a short-path apparatus

Sources & evidence

ORD record: ord-d4afc4dfb59247bfba75ef724dd5e9a3
Source dataset: uspto-grants-1977_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04038312

Reaction notes

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