Water → HCID 69847485, compound

HRID 1658613Notes

Reaction equation

HRID 1658613 reaction equation
C(OCC[N:7]1[C:13]2[CH:14]=[CH:15][C:16](Cl)=[CH:17][C:12]=2[C:11]2(C3C=CC=CC=3F)OCC[N:10]2[CH2:9][C:8]1=O)(=O)C.[OH-:30].[Na+].O>CO>[N:7]1[C:13]2=[CH:14][CH2:15][CH2:16][C:17](=[O:30])[C:12]2=[CH:11][N:10]=[CH:9][CH:8]=1

Participants

5

Procedure

A solution of 0.5g (0.0012 M) of 7-(2-acetoxyethyl)-10-chloro-11b-(2-fluorophenyl)-2,3,5,11b-tetrahydrooxazolo[3,2-d] [1,4]benzodiazepin-6(7H)-one in 5 ml of methanol was treated with 2 ml of 3N sodium hydroxide. After 3 hours, 50 ml of water was added and the solution was extracted with 40 ml of dichloromethane, which was then dried over anhydrous sodium sulfate and evaporated to dryness. The residue was crystallized from a mixture of methanol and water to give 10-chloro-11b-(2-fluorophenyl)-7-(2-hydroxyethyl)-2,3,5,11b-tetrahydrooxazolo)3,2-d) [1,4]benzodiazepin-6(7H)-one as white prisms, m.p. and m.m.p. 141°-146°.

Workup

  1. extractionthe solution was extracted with 40 ml of dichloromethane, which
  2. dry with materialwas then dried over anhydrous sodium sulfate
  3. customevaporated to dryness
  4. customThe residue was crystallized from a mixture of methanol and water

Sources & evidence

ORD record
ord-7f1e31fcfea64ea7826bebca272da043
Source dataset
uspto-grants-1976_06
Patent number
US03965151

Reaction notes

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