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Ethylmorpholine → HCID 20487949、化合物

HRID 1995744
ノート
印刷プレビュー

反応式

HRID 1995744 の反応式
Cl.[C:2]([CH:6]1[CH:11]2[CH2:12][CH:8]([CH2:9][CH2:10]2)[NH:7]1)([O:4][CH3:5])=[O:3].[C:13]([CH2:17][CH2:18][CH:19]([CH3:23])[C:20](O)=[O:21])([O:15][CH3:16])=[O:14].C(N1CCOCC1)C.ON1C2C=CC=CC=2N=N1.C1(N=C=NC2CCCCC2)CCCCC1>C(OCC)(=O)C.O1CCCC1>[C:2]([CH:6]1[CH:11]2[CH2:12][CH:8]([CH2:9][CH2:10]2)[N:7]1[C:20](=[O:21])[CH:19]([CH3:23])[CH2:18][CH2:17][C:13]([O:15][CH3:16])=[O:14])([O:4][CH3:5])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 7525EthylmorpholineHCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 131928974-Carbomethoxy-2-methylbutanoic acidHCID 20487957Methyl 2-azabicyclo[2.2.1]heptane-3-carboxylate hydrochloride

生成物 1

HCID 20487949HCID 20487949、化合物収率 57.4%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 3.83 g (0.02 m) of 3-carbomethoxy-2-azabicyclo[2.2.1]heptane hydrochloride from Example 1, 3.29 g (0.02 m) of 4-carbomethoxy-2-methylbutanoic acid, 2.3 g of N-ethylmorpholine, 5.4 g of 1-hydroxybenzotriazole, 4.13 g of dicyclohexylcarbodiimide and 60 ml of dry tetrahydrofuran was prepared with cooling and stirring, then, allowed to stir at room temperature for 18 hours. The mixture was filtered. The filtrate was evaporated to give a syrup which was dissolved in ethyl acetate and washed with 10% acetic acid/water and water. A solid separated. The ethyl acetate extract was further washed with 5% sodium bicarbonate solution and brine, then, dried and evaporated under reduced pressure to give 3.41 g (57%) of 3-carbomethoxy-2-(4-carbomethoxy-2-methylbutanoyl)-2-azabicyclo[2.2.1]heptane, mE 297.

後処理

  1. customwas prepared
  2. temperaturewith cooling
  3. stirringto stir at room temperature for 18 hours
  4. filtrationThe mixture was filtered
  5. customThe filtrate was evaporated
  6. customto give a syrup which
  7. washwashed with 10% acetic acid/water and water
  8. customA solid separated
  9. extractionThe ethyl acetate extract
  10. washwas further washed with 5% sodium bicarbonate solution and brine
  11. customdried
  12. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-83a1bb81f19b4c309f8086510a1c8229
出典データセット
uspto-grants-1983_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04405787

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート