Hydrochloric Acid → 4-Aminotetrahydro-2H-pyran-4-carboxylic acid ethyl ester

HRID 2288105노트

반응식

HRID 2288105 반응식
[CH2:1]([O:3][C:4]([C:6]1([N:12]=C(C2C=CC=CC=2)C2C=CC=CC=2)[CH2:11][CH2:10][O:9][CH2:8][CH2:7]1)=[O:5])[CH3:2].Cl>C(OCC)C>[CH2:1]([O:3][C:4]([C:6]1([NH2:12])[CH2:7][CH2:8][O:9][CH2:10][CH2:11]1)=[O:5])[CH3:2]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 545353934-[N-(diphenylmethylene)amino]tetrahydropyran-4-carboxylic acid ethyl ester

생성물 1

HCID 544950714-Aminotetrahydro-2H-pyran-4-carboxylic acid ethyl ester수율 87.6%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a solution of 4-[N-(diphenylmethylene)amino]tetrahydropyran-4-carboxylic acid ethyl ester (16.0 grams, 0.047 mole) in diethyl ether (120 mL) was added 1M aqueous hydrochloric acid solution (100 mL). The mixture was stirred vigorously at room temperature for 16 hours. The layers were separated and the aqueous layer washed with diethyl ether. The aqueous layer was brought to pH 10 with dilute aqueous ammonium hydroxide solution and extracted with dichloromethane. The organic extract was dried over sodium sulfate and concentrated to give 4-aminotetrahydropyran-4-carboxylic acid ethyl ester (7.128 g, 71.7%) as an oil.

후처리

  1. customThe layers were separated
  2. washthe aqueous layer washed with diethyl ether
  3. extractionextracted with dichloromethane
  4. extractionThe organic extract
  5. dry with materialwas dried over sodium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-006e6c7fd2884c88aaa00e10bfeecd26
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06087392

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