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Hydrochloric Acid → HCID 12765184, compound

HRID 2353089
Notes
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Reaction equation

HRID 2353089 reaction equation
[C:1]([C:4]1([C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH2:9][CH2:8][C:7](=[O:10])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[CH:16](OC)(OC)OC.Cl>CO>[CH3:16][O:10][C:7]12[CH2:8][CH2:9][C:4]([C:11]([O:13][CH2:14][CH3:15])=[O:12])([CH2:5][CH2:6]1)[C:1](=[O:3])[CH2:2]2
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 9005Trimethyl orthoformateHCID 12522245Ethyl 1-acetyl-4-oxocyclohexane-1-carboxylate

Product 1

HCID 12765184HCID 12765184, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
5 °C

Procedure

To a stirred solution of Step 3 product (1 eq) and trimethyl orthoformate (4.00 eq) in MeOH (9.4 v/w) at 5° C. was bubbled HCl gas (approximately 5 eq) over 2 hours, maintaining a pot temperature of 5° C. Upon complete addition, the reaction mixture, under nitrogen, was heated to, and stirred at, reflux for 30 minutes.

Workup

  1. additionUpon complete addition
  2. temperaturethe reaction mixture, under nitrogen, was heated to, and
  3. temperaturereflux for 30 minutes

Sources & evidence

ORD record
ord-e03d5a6aebe04bcc8d27c969e6a696aa
Source dataset
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07749997B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes