Lithium hydroxide, monohydrate → HCID 59186045, compound

HRID 1671336Notes

Reaction equation

HRID 1671336 reaction equation
C([O:3][C:4]([C:6]1[C:7]([CH2:23][CH3:24])=[N:8][N:9]2[C:13]([C:14]3[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=3[Cl:21])=[C:12]([CH3:22])[O:11][C:10]=12)=[O:5])C.O.[OH-].[Li+].CO.O>O.C(O)(=O)C>[Cl:21][C:15]1[CH:16]=[C:17]([Cl:20])[CH:18]=[CH:19][C:14]=1[C:13]1[N:9]2[N:8]=[C:7]([CH2:23][CH3:24])[C:6]([C:4]([OH:5])=[O:3])=[C:10]2[O:11][C:12]=1[CH3:22]

Participants

6

Reactant 3

HCID 168937Lithium hydroxide, monohydrateHCID 22242641Methanol--water (1/1)HCID 67212485HCID 67212485, compound

Product 1

HCID 59186045HCID 59186045, compound

Reagents, catalysts & solvents 2

HCID 176Acetic AcidSolventHCID 962WaterSolvent

Procedure

A suspension containing 3-(2,4-dichloro-phenyl)-6-ethyl-2-methyl-pyrazolo[5,1-b]oxazole-7-carboxylic acid ethyl ester (1.80 g, 4.90 mmol) and lithium hydroxide monohydrate (1.0 g, 24.51 mmol) is heated at 70° C. in a 3/1 mixture of methanol/water (32 ml) for 2 hrs. The resulting solution is cooled to RT, diluted with water (60 ml) and glacial acetic acid added (approx. 3 ml) to adjust the pH to 4-5. The resultant suspension is stirred for 1 h and filtered and washed with water. The product is dried in vacuo at 50° C.; MS: m/z 339.03 [M+H]+

Workup

  1. additionadded (approx. 3 ml)
  2. filtrationfiltered
  3. washwashed with water
  4. customThe product is dried in vacuo at 50° C.

Sources & evidence

ORD record
ord-66ea944059a84db8b7208e8ff19d739f
Source dataset
uspto-grants-2011_08
Patent number
US07994203B2

Reaction notes

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