Ammonium Hydroxide → HCID 13059436, compound

HRID 223371Notes

Reaction equation

HRID 223371 reaction equation
Cl.[O:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][CH2:4][CH:3]1[CH2:12][CH2:13][N:14]1[CH2:25][CH2:24][C:17]2([O:22][CH2:21][C:20](=[O:23])[NH:19][CH2:18]2)[CH2:16][CH2:15]1.[OH-].[NH4+]>O>[O:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][CH2:4][CH:3]1[CH2:12][CH2:13][N:14]1[CH2:25][CH2:24][C:17]2([O:22][CH2:21][C:20](=[O:23])[NH:19][CH2:18]2)[CH2:16][CH2:15]1

Participants

4

Reactant 2

HCID 14923Ammonium HydroxideHCID 205221169-[2-(1,4-Benzodioxan-2-yl)ethyl]-1-oxa-4,9-diazaspiro[5.5]undecan-3-one hydrochloride salt

Product 1

HCID 13059436HCID 13059436, compoundYield 95.1%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A solution of 3.5 g of 9-[2-(1,4-benzodioxan-2-yl)ethyl]-1-oxa-4,9-diazaspiro[5.5]undecan-3-one hydrochloride salt in water (50 ml) was adjusted to pH 12 with ammonium hydroxide solution and extracted with methylene chloride. The methylene chloride was evaporated to afford 3 g of 9-[2-(1,4-benzodioxan-2-yl)ethyl]-1-oxa-4,9-diazaspiro-[5.5]undecan-3-one as the free base, mp 139°-140° C.

Workup

  1. extractionextracted with methylene chloride
  2. customThe methylene chloride was evaporated

Sources & evidence

ORD record
ord-19ed51f29bce4adfb58d446bdfef0647
Source dataset
uspto-grants-1982_10
Patent number
US04353901

Reaction notes

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