Isopropanol → HCID 13784149, compound

HRID 570002Notes

Reaction equation

HRID 570002 reaction equation
[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:19]=[C:18](Cl)[C:17]([CH2:21][C:22]([O:24]CC)=O)=[CH:16][N:15]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:27]([NH2:29])[CH3:28].C(O)(C)C>O>[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:15]=[CH:16][C:17]3[CH2:21][C:22](=[O:24])[N:29]([CH2:27][CH3:28])[C:18]=3[N:19]=2)[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

5

Reactant 3

HCID 3776IsopropanolHCID 6341EthylamineHCID 13784183HCID 13784183, compound

Product 1

HCID 13784149HCID 13784149, compoundYield 46%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
120 °C

Procedure

A mixture of 1.41 g (3.76 mmol, Referential Example 71) of ethyl 2-(4-benzylpiperazino)-4-chloropyrimidine-5-acetate, 5 ml of ethylamine and 20 ml of isopropanol was placed in a pressure vessel, in which they were heated at 120° C. for 2 hours. The solvent was then driven off under reduced pressure. The residue was added with water, followed by extraction with chloroform. After drying the organic layer with MgSO4, it was concentrated. The residue was purified by silica gel column chromatography to obtain 0.58 of the above-identified compound (yield: 46%).

Workup

  1. customwas placed in a pressure vessel, in which they
  2. extractionfollowed by extraction with chloroform
  3. dry with materialAfter drying the organic layer with MgSO4, it
  4. concentrationwas concentrated
  5. customThe residue was purified by silica gel column chromatography

Sources & evidence

ORD record
ord-fb9c55e7edc3483b8d946c2e64b80479
Source dataset
uspto-grants-1988_03
Patent number
US04734418

Reaction notes

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