Hydrochloric Acid → HCID 58684179、化合物

HRID 40544ノート

反応式

HRID 40544 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 58684179HCID 58684179、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7da3d1ff0ec84e8daa09d87bc8dbb7e3
出典データセット
uspto-grants-2013_09
特許番号
US08530473B2

反応ノート

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