Hydrochloric Acid → HCID 58684179, 화합물

HRID 40544노트

반응식

HRID 40544 반응식
[C:1]([O:5][N:6]=[C:7]1[CH2:12][CH2:11][N:10](C(O)=O)[CH2:9][CH2:8]1)([CH3:4])([CH3:3])[CH3:2].Cl.O1CCOCC1.C(=O)([O-])O.[Na+]>ClCCl>[C:1]([O:5][N:6]=[C:7]1[CH2:8][CH2:9][NH:10][CH2:11][CH2:12]1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 516892Sodium BicarbonateHCID 230330724-Tert-butoxyimino-piperidine-1-carboxylic acid

생성물 1

HCID 58684179HCID 58684179, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 34 ml of dichloromethane containing 0.9 g of tert-butyl ester of 4-tert-butoxyimino-piperidine-1-carboxylic acid is cooled to 0° C. 25 ml of a 4M solution of hydrochloric acid in dioxane (30 eq) is added. The reaction mixture is stirred at room temperature for 3 hours and then diluted by adding dichloromethane. A saturated solution of sodium hydrogen carbonate is then added until pH=8 is obtained. The aqueous phase is extracted three times with dichloromethane. The organic phases are then combined, dried over sodium sulfate, filtered and concentrated to dryness under reduced pressure. 0.49 g of piperidin-4-one O-tert-butyl-oxime is obtained.

후처리

  1. additiondiluted
  2. customis obtained
  3. extractionThe aqueous phase is extracted three times with dichloromethane
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-7da3d1ff0ec84e8daa09d87bc8dbb7e3
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530473B2

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