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

HRID 2288105ノート

反応式

HRID 2288105 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-006e6c7fd2884c88aaa00e10bfeecd26
出典データセット
uspto-grants-2000_07
特許番号
US06087392

反応ノート

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