Isopropylamine → HCID 21413140, compound

HRID 2071243Notes

Reaction equation

HRID 2071243 reaction equation
[C:1]1([CH:7]2[CH:12]([C:13]([OH:15])=O)[O:11][C:10]3[CH:16]=[CH:17][CH:18]=[CH:19][C:9]=3[O:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)(Cl)(Cl)Cl.[CH:26]([NH2:29])([CH3:28])[CH3:27]>C1C=CC=CC=1>[CH:26]([NH:29][C:13]([CH:12]1[O:11][C:10]2[CH:16]=[CH:17][CH:18]=[CH:19][C:9]=2[O:8][CH:7]1[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)=[O:15])([CH3:28])[CH3:27]

Participants

5

Reactant 3

HCID 6363IsopropylamineHCID 24819Phosphorus pentachlorideHCID 12748779HCID 12748779, compound

Product 1

HCID 21413140HCID 21413140, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent2×

Procedure

To 22 g of (3-phenyl-1,4-benzodioxan-2-yl)-carboxylic acid in 300 cc of anhydrous benzene are added 18.1 g of PCl5 in portions with cooling. After 2 hours the reaction mixture is added to a cold solution of isopropylamine in anhydrous benzene. After stirring for 2 hours, the product is poured onto ice. The organic phase is separated, washed with H2O and finally dried over Na2SO4. The solvent is removed under vacuum. The residue is crystallised from isopropyl alcohol, m.p. = 196°-8°.

Workup

  1. temperaturewith cooling
  2. additionthe product is poured onto ice
  3. customThe organic phase is separated
  4. washwashed with H2O
  5. dry with materialfinally dried over Na2SO4
  6. customThe solvent is removed under vacuum
  7. customThe residue is crystallised from isopropyl alcohol, m.p. = 196°-8°

Sources & evidence

ORD record
ord-336f9ced930f4532947ce36c898be86d
Source dataset
uspto-grants-1977_09
Patent number
US04046762

Reaction notes

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