Water → 4-Piperidino-2,6-lutidine-1-oxide

HRID 1764104노트

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HRID 1764104 반응식
Cl.Cl[C:3]1[CH:4]=[C:5]([CH3:11])[N+:6]([O-:10])=[C:7]([CH3:9])[CH:8]=1.[NH:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1.O>C(Cl)(Cl)Cl>[N:12]1([C:3]2[CH:4]=[C:5]([CH3:11])[N+:6]([O-:10])=[C:7]([CH3:9])[CH:8]=2)[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1

참가 물질

5

반응물 3

HCID 962Water2회HCID 8082PiperidineHCID 227642674-Chloro-2,6-lutidine-1-oxide hydrochloride

생성물 1

HCID 227642734-Piperidino-2,6-lutidine-1-oxide수율 50%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
25 °C

실험 절차

A quantity (1.94 g., 0.01 mole) of 4-chloro-2,6-lutidine-1-oxide hydrochloride with 6 ml. piperidine, and 10 ml. water were sealed in a reinforced bottle and heated, with stirring, in an oil bath at the temperature 155° to 160° C. for 41/2 hrs. After cooling the reaction mixture to 25° C. and diluting it with 25 ml. water, several portions of chloroform were used to extract the objective product. The chloroform extracts were combined, dried over anhydrous sodium sulfate, treated with charcoal, and filtered. The filtrate was pale yellow. The chloroform was removed by evaporation under reduced pressure. The solid residue thus obtained was triturated with technical hexane (Skellysolve B, a mixture of isomeric hexanes having a boiling range between 142° and 156° F.) and then crystallized from about 10 ml. ethyl acetate. There was thus obtained 1.06 g. (50% yield) of 4-piperidino-2,6-lutidine-1-oxide as buff-colored crystals having a melting point at 87° to 90° C.

후처리

  1. temperatureheated
  2. additiondiluting it with 25 ml
  3. extractionto extract the objective product
  4. dry with materialdried over anhydrous sodium sulfate
  5. additiontreated with charcoal
  6. filtrationfiltered
  7. customThe chloroform was removed by evaporation under reduced pressure
  8. customThe solid residue thus obtained
  9. customwas triturated with technical hexane (Skellysolve B
  10. additiona mixture of isomeric hexanes having a boiling range between 142° and 156° F.) and
  11. customthen crystallized from about 10 ml

출처 및 근거

ORD 기록
ord-ba0d4949a03f49a1813f63952b59b33d
출처 데이터셋
uspto-grants-1978_09
특허 번호
US04115396

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