HCID 67582513, compound → HCID 15859426, compound

HRID 1416413Notes

Reaction equation

HRID 1416413 reaction equation
Br.[CH2:2]([C:4]1[S:8][C:7](=[NH:9])[N:6]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]#[N:24])=[CH:13][CH:12]=2)[N:5]=1)[CH3:3]>C(Cl)(Cl)Cl.[OH-].[Na+]>[CH2:2]([C:4]1[S:8][C:7](=[NH:9])[N:6]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]#[N:24])=[CH:13][CH:12]=2)[N:5]=1)[CH3:3]

Participants

4

Reactant 1

HCID 67582513HCID 67582513, compound

Product 1

HCID 15859426HCID 15859426, compoundYield 93.6%

Reagents, catalysts & solvents 2

HCID 6212ChloroformSolventHCID 14798Sodium HydroxideSolvent

Procedure

To a suspension of 4.0 g of 5-ethyl-2-imino-3-(2'-cyanobiphenyl-4-yl)methyl-1,3,4-thiadiazoline.hydrobromide in 60 ml of chloroform, 10 ml of 2N sodium hydroxide was added, followed by stirring at room temperature for one hour. After separation, the organic layer was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The resulting oil was crystallized from n-hexane, whereby 2.99 g of the title compound was obtained.

Workup

  1. additionwas added
  2. customAfter separation
  3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting oil was crystallized from n-hexane

Sources & evidence

ORD record
ord-6f11fa42fd294b38b05fe48115300ca7
Source dataset
uspto-grants-1999_06
Patent number
US05912353

Reaction notes

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