Hydrogen chloride-ethyl acetate → HCID 68581637, compound

HRID 2237600Notes

Reaction equation

HRID 2237600 reaction equation
[CH2:1]([O:3][C:4]([C:6]1[N:15]=[C:14]([NH:16][C@H:17]2[CH2:22][CH2:21][CH2:20][CH2:19][C@H:18]2[NH:23]C(OC(C)(C)C)=O)[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([CH3:31])[CH:12]=2)[N:7]=1)=[O:5])[CH3:2].C(OCC)(=O)C.[ClH:38]>C(OCC)(=O)C>[ClH:38].[ClH:38].[CH2:1]([O:3][C:4]([C:6]1[N:15]=[C:14]([NH:16][C@H:17]2[CH2:22][CH2:21][CH2:20][CH2:19][C@H:18]2[NH2:23])[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([CH3:31])[CH:12]=2)[N:7]=1)=[O:5])[CH3:2]

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 68581553HCID 68581553, compound

Product 1

HCID 68581637HCID 68581637, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

To a solution of 14.5 g of 4-({(1S,2R)-2-[(tert-butoxycarbonyl)amino]cyclohexyl}amino)-6-methylquinazoline-2-carboxylic acid ethyl ester in 600 ml of ethyl acetate, 68 ml of a 4N-hydrogen chloride-ethyl acetate solution was added under ice cooling, and then the mixture was stirred at room temperature for 11 hours. The deposited crystals were collected by filtration, washed with ethyl acetate and then dried to obtain 11.7 g of the desirable compound as a pink powder.

Workup

  1. filtrationThe deposited crystals were collected by filtration
  2. washwashed with ethyl acetate
  3. customdried

Sources & evidence

ORD record
ord-fea2fe2abbd544e38f9e72e4227432a8
Source dataset
uspto-grants-2010_05
Patent number
US07718663B2

Reaction notes

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