Hydrochloric Acid → HCID 19930842、化合物

HRID 5411ノート

反応式

HRID 5411 の反応式
[O:1]=[C:2]1[CH:15]([C:16]([O:18]CC)=[O:17])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH:4]([C:21]([O:23]CC)=[O:22])[NH:3]1.[OH-].[Na+].Cl>C(O)C>[O:1]=[C:2]1[CH:15]([C:16]([OH:18])=[O:17])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH:4]([C:21]([OH:23])=[O:22])[NH:3]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 19930817Diethyl 2-oxo-1-azacyclotetradecane-3,14-dicarboxylate

生成物 1

HCID 19930842HCID 19930842、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Diethyl 2-oxo-1-azacyclotetradecane-3,14-dicarboxylate (1.14 g, 3.2 mmol; mixture of both diastereomers) is dissolved in ethanol (32.0 mL). Sodium hydroxide (9.6 mL of a 1N aqueous solution, 9.6 mmol) is added dropwise, and the solution is stirred at room temperature for 3 hours. The reaction is then acidified to pH 3 with 1N hydrochloric acid, and partitioned between ethyl acetate and water. The aqueous phase is extracted several times with ethyl acetate, the combined organic layers are dried (Na2SO4), and the solvent is evaporated to give both diastereomers of 2-oxo-1-azacyclotetradecane-3,14-dicarboxylic acid.

後処理

  1. additionmixture of both diastereomers)
  2. custompartitioned between ethyl acetate and water
  3. extractionThe aqueous phase is extracted several times with ethyl acetate
  4. dry with materialthe combined organic layers are dried (Na2SO4)
  5. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-951c6a1597cb49a28e3182feddd4d406
出典データセット
uspto-grants-1993_09
特許番号
US05244889

反応ノート

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