Diethyl Ether → HCID 18980435, compound

HRID 2392768Notes

Reaction equation

HRID 2392768 reaction equation
[O:1]1[C:5]2([CH2:10][CH2:9][C:8](=[O:11])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.C(Cl)[Cl:13].[CH3:15][NH2+:16][CH3:17].[C:18](Cl)(=O)C.CCOCC>C(#N)C>[ClH:13].[CH3:15][N:16]([CH2:18][CH:9]1[C:8](=[O:11])[CH2:7][CH2:6][C:5]2([O:4][CH2:3][CH2:2][O:1]2)[CH2:10]1)[CH3:17]

Participants

6

Reactant 4

HCID 3283Diethyl EtherHCID 6367Acetyl chlorideHCID 5674151,4-Dioxaspiro[4.5]decan-8-oneHCID 22610303HCID 22610303, compound

Product 1

HCID 18980435HCID 18980435, compoundYield 98%

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

130 g (0.83 mole) 1,4-dioxa-spiro[4.5]-decan-8-one and 79.5 g (0.83 mole) dimethylammonium methylene chloride were stirred in 500 ml acetonitrile at room temperature. After adding 1 ml acetyl chloride, the mixture was stirred for 3 hours at room temperature, whereupon a clear, colourless solution was formed. 1 litre ether was then added drop-wise to the reaction mixture. 203 g (98% theoretical) 7-dimethylaminomethyl-1,4-dioxa-spiro[4.5]decan-8-one hydrochloride (64) were obtained in crystalline form.

Workup

  1. customwhereupon a clear, colourless solution was formed

Sources & evidence

ORD record
ord-7c747e0d695a4b81af332f374cf849c4
Source dataset
uspto-grants-1998_09
Patent number
US05801201

Reaction notes

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