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Morpholine → 2-(Morpholine-4-carbonyl)cyclohexane-1-carboxylic acid

HRID 427392
ノート
印刷プレビュー

反応式

HRID 427392 の反応式
[C@@H:1]12[C:10](=[O:11])[O:9][C:7](=[O:8])[C@@H:2]1[CH2:3][CH2:4][CH2:5][CH2:6]2.[NH:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1>C(Cl)Cl>[N:12]1([C:7]([CH:2]2[CH2:3][CH2:4][CH2:5][CH2:6][CH:1]2[C:10]([OH:9])=[O:11])=[O:8])[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8083MorpholineHCID 641660Hexahydrophthalic anhydride, cis-

生成物 1

HCID 31145632-(Morpholine-4-carbonyl)cyclohexane-1-carboxylic acid収率 90%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of cis-1,2-cyclohexane dicarboxylic anhydride (1.0 g, 6.49 mmol) in CH2Cl2 (16 mL) was added morpholine (0.56 g, 6.49 mmol) at 0° C., the resulting mixture was allowed to stir at room temperature overnight (20 h). When complete the reaction mixture was washed with HCl (1.0 N, 20 mL) then with H2O (2×20 mL). The combined aqueous layers were extracted with CH2Cl2 (3×10 mL), and the combined organic layers were dried over MgSO4, the solvent was evaporated in vacuo to give the title compound (1.4 g, 90%/) as a white solid which was used later without further purification.

後処理

  1. washWhen complete the reaction mixture was washed with HCl (1.0 N, 20 mL)
  2. extractionThe combined aqueous layers were extracted with CH2Cl2 (3×10 mL)
  3. dry with materialthe combined organic layers were dried over MgSO4
  4. customthe solvent was evaporated in vacuo

出典と根拠

ORDレコード
ord-ddbeeefd8af747ce8d0a080bcde97eae
出典データセット
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06313117B1

反応ノート

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