HCID 13519550, compound → HCID 13519549, compound

HRID 371143Notes

Reaction equation

HRID 371143 reaction equation
Br.[Cl:2][C:3]1[CH:4]=[C:5]([C:10]23[CH:18]4[CH2:19][CH:15]([CH2:16][CH2:17]4)[CH:14]2[CH2:13][NH:12][CH2:11]3)[CH:6]=[CH:7][C:8]=1[Cl:9]>O>[ClH:2].[Cl:2][C:3]1[CH:4]=[C:5]([C:10]23[CH:18]4[CH2:19][CH:15]([CH2:16][CH2:17]4)[CH:14]2[CH2:13][NH:12][CH2:11]3)[CH:6]=[CH:7][C:8]=1[Cl:9]

Participants

3

Reactant 1

HCID 13519550HCID 13519550, compound

Product 1

HCID 13519549HCID 13519549, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

An 0.8 g amount of the above hydrobromide was dissolved in 250 ml of hot water, then filtered. The filtrate was made basic with 10N sodium hydroxide and extracted with both dichloromethane and ether. The combined organic solutions were dried over anhydrous sodium sulfate and evaporated in vacuo to give0.35 g of a viscous liquid. This liquid was dissolved in ether and acidified with anhydrous hydrogen chloride to form a solid. The solid was collected and recrystallized from ethanol hexane to give 0.11 g of the product of the Example as gray crystals, mp 246°-248° C. (dec.).

Workup

  1. filtrationfiltered
  2. extractionextracted with both dichloromethane and ether
  3. dry with materialThe combined organic solutions were dried over anhydrous sodium sulfate
  4. customevaporated in vacuo to give0
  5. dissolutionThis liquid was dissolved in ether
  6. customto form a solid
  7. customThe solid was collected
  8. customrecrystallized from ethanol hexane

Sources & evidence

ORD record
ord-8eb58fc5dc504a31b09e39c844111091
Source dataset
uspto-grants-1985_07
Patent number
US04529736

Reaction notes

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