Phosphoric Acid → HCID 20357924, compound

HRID 2083177Notes

Reaction equation

HRID 2083177 reaction equation
[P:1](=[O:5])([OH:4])([OH:3])[OH:2].C([N:8]([CH2:11][CH3:12])[CH2:9][CH3:10])C.[CH3:13][Si:14]([CH3:19])([CH3:18])[CH2:15][CH2:16]O.Cl[C:21](Cl)(Cl)[C:22]#N.[CH:26]1(N)[CH2:31]CC[CH2:28][CH2:27]1>C(#N)C.CC(C)=O>[CH:11]1([NH2+:8][CH:9]2[CH2:10][CH2:16][CH2:15][CH2:22][CH2:21]2)[CH2:12][CH2:28][CH2:27][CH2:26][CH2:31]1.[P:1]([OH:4])([OH:3])([O:2][CH2:16][CH2:15][Si:14]([CH3:19])([CH3:18])[CH3:13])=[O:5]

Participants

8

Reactant 5

HCID 1004Phosphoric AcidHCID 7965CyclohexylamineHCID 8471TriethylamineHCID 11011TrichloroacetonitrileHCID 180132-(Trimethylsilyl)ethanol

Product 1

HCID 20357924HCID 20357924, compound

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 6342AcetonitrileSolvent

Procedure

A solution in acetonitrile (30 ml) of crystalline phosphoric acid (2.0 g) and triethylamine (4.0 g) was added dropwise over 4 hours to a mixture of 2-(trimethylsilyl)-ethanol (3.0 g) and and trichloroacetonitrile (8.6 g) at room temperature. The mixture was left overnight, diluted with acetone (200 ml) and cyclohexylamine (15 ml) was added. The precipitate was collected and recrystallised from water and then ethanol 10% cyclohexylamine to give the cyclohexylammonium salt, (1.3 g) m.p. 252°-255°.

Workup

  1. additionwas added
  2. customThe precipitate was collected
  3. customrecrystallised from water

Sources & evidence

ORD record
ord-d36262910ae048e8b4362b7aed4eb1a8
Source dataset
uspto-grants-1978_04
Patent number
US04084951

Reaction notes

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