Hydrochloric Acid → HCID 67699230, compound

HRID 482327Notes

Reaction equation

HRID 482327 reaction equation
[O:1]=[C:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[CH2:8][CH2:9][N:10]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12]2[C:19]([N:28]3[CH2:32][CH2:31][CH2:30][CH2:29]3)=[N:20][C:21]([N:23]3[CH2:27][CH2:26][CH2:25][CH2:24]3)=[N:22][C:11]1=2.[ClH:33]>C(O)C>[ClH:33].[O:1]=[C:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[CH2:8][CH2:9][N:10]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12]2[C:19]([N:28]3[CH2:32][CH2:31][CH2:30][CH2:29]3)=[N:20][C:21]([N:23]3[CH2:24][CH2:25][CH2:26][CH2:27]3)=[N:22][C:11]1=2

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 53966265HCID 53966265, compound

Product 1

HCID 67699230HCID 67699230, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A hot solution of 9-[2--(3-Oxo-4-morpholinyl)ethyl]-2,4-di-1-pyrrolidinyl-9H-pyrimido[4,5-b]indole (XIII, EXAMPLE30, 0.91 g, 2.1 mmol) in ethanol (60 mL) is treated with aqueous hydrochloric acid (5M, 0.43 mL, 2.15 mmol). The mixture is cooled to 20°-250° and concentrated under reduced pressure to a solid. Recrystallization of the solid from acetone/methanol/ether gives the title compound, mp=210°-213°; IR (mull) 1651, 1631, 1573, 1554, 1527, 1499, 1486, 1436, 1415, 1353, 1339, 1312, 1241, 1110 and 772 cm-1. ##STR9##

Workup

  1. temperatureThe mixture is cooled to 20°-250°
  2. concentrationconcentrated under reduced pressure to a solid
  3. customRecrystallization of the solid from acetone/methanol/ether

Sources & evidence

ORD record
ord-1c97bf93d17240c1bdee0daefe4b8894
Source dataset
uspto-grants-1998_08
Patent number
US05795986

Reaction notes

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