Ammonium Hydroxide → HCID 18607003, compound

HRID 1906411Notes

Reaction equation

HRID 1906411 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][C:10]2[C:21]3[C:26]([CH:27]=[CH:28][C:9]=2[N:8]([CH2:29][CH2:30][N:31]([CH2:34][CH3:35])[CH2:32][CH3:33])[C:7]1=[O:36])=[CH:25][CH:24]=[CH:23][CH:22]=3)(=[O:4])[CH3:3].[OH-].[NH4+]>O>[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][C:10]2[C:21]3[C:26]([CH:27]=[CH:28][C:9]=2[N:8]([CH2:29][CH2:30][N:31]([CH2:32][CH3:33])[CH2:34][CH3:35])[C:7]1=[O:36])=[CH:25][CH:24]=[CH:23][CH:22]=3)(=[O:4])[CH3:3]

Participants

4

Reactant 2

HCID 14923Ammonium HydroxideHCID 18607010HCID 18607010, compound

Product 1

HCID 18607003HCID 18607003, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A sample of the above hydrochloride, in water was treated with concentrated ammonium hydroxide and the aqueous suspension was extracted with ether. The ether solutions were washed with water and dried (magnesium sulfate). Removal of the solvent gave the base, which after crystallization from ether afforded (±)-cis-3-(acetyloxy)-5-[2-(diethylamino)ethyl]-2,3-dihydro-2-(4-methoxyphenyl)naphtho[1,2-b]-1,4-thiazepin-4(5H)-one, mp 148°-149°.

Workup

  1. extractionthe aqueous suspension was extracted with ether
  2. washThe ether solutions were washed with water
  3. dry with materialdried (magnesium sulfate)
  4. customRemoval of the solvent
  5. customgave the base, which
  6. customafter crystallization from ether

Sources & evidence

ORD record
ord-7fb1989ab2e149129fdd6c1b79a23dbd
Source dataset
uspto-grants-1987_03
Patent number
US04652561

Reaction notes

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