Hydrochloric Acid → HCID 21490901, 화합물

HRID 1973903노트

반응식

HRID 1973903 반응식
Cl.[K].[C:3]([C:6]1[CH:11]=[C:10]([Cl:12])[C:9]([CH2:13][CH2:14][CH2:15][CH3:16])=[C:8]([Cl:17])[N:7]=1)([OH:5])=[O:4].[CH3:18]O>>[CH3:18][O:4][C:3]([C:6]1[CH:11]=[C:10]([Cl:12])[C:9]([CH2:13][CH2:14][CH2:15][CH3:16])=[C:8]([Cl:17])[N:7]=1)=[O:5]

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 5462222PotassiumHCID 21490880HCID 21490880, 화합물

생성물 1

HCID 21490901HCID 21490901, 화합물

실험 절차

300 ml of 5 N hydrochloric acid in methanol are added to 28.6 g (0.1 mol) of the potassium salt of 2-carboxy-4,6-dichloro-5-n-butyl-pyridine and the mixture is heated for 8 hours under reflux. It is then evaporated to dryness and hydrochloric acid which still adheres is distilled off with toluene. The residue is rendered alkaline with 2 N sodium carbonate solution and extracted with ether. The ether phases are combined, dried with sodium sulphate and evaporated. Distillation of the residue in a bulb tube at a temperature of 140°-160° at 0.3 mm Hg yields 2-methoxycarbonyl-4,6-dichloro-5-n-butyl-pyridine of the formula ##STR31##

후처리

  1. temperaturethe mixture is heated for 8 hours
  2. temperatureunder reflux
  3. customIt is then evaporated to dryness and hydrochloric acid which
  4. distillationstill adheres is distilled off with toluene
  5. extractionextracted with ether
  6. dry with materialdried with sodium sulphate
  7. customevaporated
  8. distillationDistillation of the residue in a bulb tube at a temperature of 140°-160° at 0.3 mm Hg

출처 및 근거

ORD 기록
ord-063305cf5cb84c39b55c9ecf63a9dda3
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03998955

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