Ammonium Hydroxide → HCID 15093148, compound

HRID 981469Notes

Reaction equation

HRID 981469 reaction equation
Cl.[C:2]([O:5][C@H:6]1[C@@H:12]([C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=2)[S:11][CH:10]=[C:9]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[N:8]([CH2:27][CH2:28][N:29]([CH3:31])[CH3:30])[C:7]1=[O:32])(=[O:4])[CH3:3].[OH-].[NH4+]>O>[C:2]([O:5][C@H:6]1[C@@H:12]([C:13]2[CH:14]=[CH:15][C:16]([O:19][CH3:20])=[CH:17][CH:18]=2)[S:11][CH:10]=[C:9]([C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[N:8]([CH2:27][CH2:28][N:29]([CH3:30])[CH3:31])[C:7]1=[O:32])(=[O:4])[CH3:3]

Participants

4

Reactant 2

HCID 14923Ammonium HydroxideHCID 70083343HCID 70083343, compound

Product 1

HCID 15093148HCID 15093148, compoundYield 97%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

The above hydrochloride, 4.0 g (0.008 mole) in water was treated with ammonium hydroxide and the aqueous suspension was extracted with methylene chloride. The methylene chloride solutions were dried (MgSO4) and removal of the solvent gave 3.6 g (97%) of rac.-cis-6-(acetyloxy)-6,7-dihydro-7(4-methoxyphenyl)-4-[2-(dimethylamino)-ethyl]-3-phenyl-1 , 4-thiazepin-5(4H)-one. Analytical sample was recrystallized from ether, mp 115°-116°.

Workup

  1. extractionthe aqueous suspension was extracted with methylene chloride
  2. dry with materialThe methylene chloride solutions were dried
  3. custom(MgSO4) and removal of the solvent

Sources & evidence

ORD record
ord-80af12559e9e40b690d34b7d6510e0c4
Source dataset
uspto-grants-1991_02
Patent number
US04992432

Reaction notes

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