Hydrochloric Acid → HCID 67747011, compound

HRID 865929Notes

Reaction equation

HRID 865929 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:9][C:10](=[O:42])[NH:11][CH:12]2[C:18](=[O:19])[N:17]([CH2:20][C:21]([N:23]([CH3:30])[C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)=[O:22])[C:16]3[CH:31]=[CH:32][CH:33]=[CH:34][C:15]=3[C:14]([CH2:35][N:36]3[CH2:41][CH2:40][O:39][CH2:38][CH2:37]3)=[N:13]2)[CH:6]=[CH:7][CH:8]=1.[ClH:43]>C(Cl)Cl.C(OCC)C>[ClH:43].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:9][C:10](=[O:42])[NH:11][CH:12]2[C:18](=[O:19])[N:17]([CH2:20][C:21]([N:23]([CH3:30])[C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)=[O:22])[C:16]3[CH:31]=[CH:32][CH:33]=[CH:34][C:15]=3[C:14]([CH2:35][N:36]3[CH2:41][CH2:40][O:39][CH2:38][CH2:37]3)=[N:13]2)[CH:6]=[CH:7][CH:8]=1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 9829524HCID 9829524, compound

Product 1

HCID 67747011HCID 67747011, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 6344DichloromethaneSolvent

Procedure

A solution of the (+)-2-{3-[3-(3-Methoxy-phenyl)-ureido]-5-morpholin-4-ylmethyl 2-oxo-2,3-dihydro-benzo [e][1,4]diazepin-1-yl}-N-methyl-N-phenyl-acetamide (200 mg) in dry DCM (20 ml) under nitrogen was treated with 1M hydrogen chloride in diethyl ether (0.77 ml) and the solution was stirred for 5 min. The solvent was removed in vacuo and the residue azeotroped with toluene (2×10 ml) to give the title compound (215 mg) as a pale straw coloured solid, m.p. 160°-170° dec.

Workup

  1. customThe solvent was removed in vacuo
  2. customthe residue azeotroped with toluene (2×10 ml)

Sources & evidence

ORD record
ord-415e77bfda5c448d8d99b2039f5891a9
Source dataset
uspto-grants-1996_10
Patent number
US05569654

Reaction notes

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