Dichloromethane → HCID 86737833, compound

HRID 1680943Notes

Reaction equation

HRID 1680943 reaction equation
[N:1]1([C:7]2[N:12]=[C:11]([NH:13][C:14]([O:16][CH2:17][CH:18]([CH3:20])[CH3:19])=[O:15])[N+:10]([O-:21])=[C:9]([NH:22][C:23](OCC(C)C)=[O:24])[N:8]=2)[CH2:6][CH:5]=[CH:4][CH2:3][CH2:2]1.C(Cl)Cl.[OH-].[Na+]>O>[N:1]1([C:7]2[N:12]=[C:11]([NH:13][C:14]([O:16][CH2:17][CH:18]([CH3:20])[CH3:19])=[O:15])[N:10]3[O:21][C:23](=[O:24])[N:22]=[C:9]3[N:8]=2)[CH2:6][CH:5]=[CH:4][CH2:3][CH2:2]1

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 178452998HCID 178452998, compound

Product 1

HCID 86737833HCID 86737833, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

8 g. of diisobutyl 6-[3,6-dihydro-1(2H)-pyridyl]-s-triazine-2,4-dicarbamate-3-oxide are dissolved in 300 ml. of methylene chloride and 1000 ml. of water and adjusted to pH 12.7 with concentrated sodium hydroxide. The mixture is stirred for 75 minutes, the organic phase is separated and the aqueous phase is adjusted to pH 4 with 3-N hydrochloric acid solution. The thus-obtained acidic aqueous solution is extracted with methylene chloride. The organic extracts are dried over sodium sulfate and evaporated, there being obtained pure isobutyl 5-[3,6-dihydro-1(2H)-pyridyl]-2-oxo-2H-[1,2,4]oxadiazolo[2,3-a]-s-triazine-7-carbamate having a melting point of 210°-215° C.

Workup

  1. customthe organic phase is separated
  2. extractionThe thus-obtained acidic aqueous solution is extracted with methylene chloride
  3. dry with materialThe organic extracts are dried over sodium sulfate
  4. customevaporated

Sources & evidence

ORD record
ord-74a04336ef8f444fae83aba41ca68381
Source dataset
uspto-grants-1981_06
Patent number
US04276417

Reaction notes

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