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HCID 22875336、化合物 → rac-tert-butyl (4aR,7aS)-octahydropyrrolo[3,4-b]morpholine-6-carboxylate

HRID 2256091
ノート
印刷プレビュー

反応式

HRID 2256091 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:16][C@@H:15]2[C@@H:10]([N:11](N[C@@H](C3C=CC=CC=3)C)[CH2:12][CH2:13][O:14]2)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>[Pd].C(O)C>[C:1]([O:5][C:6]([N:8]1[CH2:16][C@@H:15]2[C@@H:10]([NH:11][CH2:12][CH2:13][O:14]2)[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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 1

HCID 22875336HCID 22875336、化合物

生成物 1

HCID 22875335rac-tert-butyl (4aR,7aS)-octahydropyrrolo[3,4-b]morpholine-6-carboxylate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒2 回HCID 702Ethanol溶媒

実験手順

A mixture of 417 mg of cis-8-tert-butoxycarbonyl-5-[(1R)-1-phenylethylamino]-2-oxa-5,8-diazabicyclo[4.3.0]nonane 14a and 200 mg of 10% palladium on charcoal in 50 ml of ethanol was shaken under a pressured hydrogen atmosphere of 4.5 kg/cm2 for 4 hours. Then further 100 mg of 10% palladium on charcoal was added and hydrogenation was carried out under the above-mentioned condition. Throughout the reaction, the reaction vessel was heated by irradiation with a tungsten lamp. The catalyst was removed by filtration, and the solvent of the filtrate was removed under reduced pressure. The residue was subjected to silica gel column chromatography. From an eluant of chloroform containing 10% methanol, the titled compound 15a weighing 286 mg was obtained.

後処理

  1. customThroughout the reaction
  2. temperaturethe reaction vessel was heated by irradiation with a tungsten lamp
  3. customThe catalyst was removed by filtration
  4. customthe solvent of the filtrate was removed under reduced pressure
  5. customwas obtained

出典と根拠

ORDレコード
ord-c0286a802d0944108910c4a8a4a43e1b
出典データセット
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05654318

反応ノート

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