Hydrochloric Acid → HCID 24872021, compound

HRID 885713Notes

Reaction equation

HRID 885713 reaction equation
Cl.C(OC([N:9]1[CH2:14][CH:13]2[CH:11]([C:12]2([CH3:16])[CH3:15])[C:10]1=[O:17])=O)(C)(C)C>C1(C)C=CC=CC=1>[CH3:15][C:12]1([CH3:16])[CH:11]2[CH:13]1[CH2:14][NH:9][C:10]2=[O:17]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 23653829HCID 23653829, compound

Product 1

HCID 24872021HCID 24872021, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

To this solution was added 569.5 g of 1% hydrochloric acid and mixed, and liquid-partitioning was caused. An organic layer obtained by liquid-partitioning was washed with 262.5 g of a 5% sodium hydrogen carbonate aqueous solution, further washed with 262.5 g of water, then, 1652.8 g of a toluene solution containing 349.7 g (1.552 mol) of 3-tert-butoxycarbonyl-6,6-dimethyl-3-azabicyclo[3.1.0]hexan-2-one was obtained. The yield with respect to 6,6-dimethyl-3-azabicyclo[3.1.0]hexan-2-one was 99.4%.

Workup

  1. additionmixed
  2. customliquid-partitioning
  3. customAn organic layer obtained
  4. customby liquid-partitioning
  5. washwas washed with 262.5 g of a 5% sodium hydrogen carbonate aqueous solution
  6. washfurther washed with 262.5 g of water
  7. customwas obtained

Sources & evidence

ORD record
ord-89a722908a264337bae0b48f16bfe098
Source dataset
uspto-grants-2012_08
Patent number
US08242285B2

Reaction notes

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