Hydrochloric Acid → HCID 22756341, compound

HRID 65921Notes

Reaction equation

HRID 65921 reaction equation
[H-].[H-].[H-].[H-].[Li+].[Al+3].[C:7]([C:12]1[CH:13]=[C:14]2[C:23]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[N:17]=[CH:16][N:15]2[CH:24]=1)(OCC)=[O:8].O.Cl>CCOCC>[OH:8][CH2:7][C:12]1[CH:13]=[C:14]2[C:23]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[NH:17][CH2:16][N:15]2[CH:24]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 4407258Ethyl pyrrolo[1,2-c]quinazoline-2-carboxylateHCID 21226445Aluminium lithium hydride

Product 1

HCID 22756341HCID 22756341, compoundYield 122.4%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

LiAlH4 (0.50 g, 0.013 m) was slurried in ether (200 ml) and to this was added a solution of the product of Example II (1.0 g, 0.007 m) in ether (50 ml). The reaction mixture was stirred at room temperature for 2 hrs. Water (30 ml) was added and the mixture was acidified with 10% HCl. The resulting mixture was extracted with ether, the ether extracts combined, dried over Na2SO4, filtered, and the solvent removed in vacuo to yield 1.02 g of a white solid. Crystallization from EtOAc/hexane afforded the product as a white solid; m.p. 128°-130° C.

Workup

  1. extractionThe resulting mixture was extracted with ether
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. customthe solvent removed in vacuo

Sources & evidence

ORD record
ord-78da900f69044c3e827010ba3c0787a0
Source dataset
uspto-grants-1978_12
Patent number
US04129653

Reaction notes

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