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Sodium Bicarbonate → HCID 15380923、化合物

HRID 610773
ノート
印刷プレビュー

反応式

HRID 610773 の反応式
[CH:1]1([NH:7][C:8](=[O:32])[CH2:9][CH2:10][CH2:11][CH2:12][N:13](CC2C=CC=CC=2)[CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[O:23][CH3:24])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(=O)([O-])O.[Na+]>C(O)(=O)C.ClCCl.[Pd]>[CH:1]1([NH:7][C:8](=[O:32])[CH2:9][CH2:10][CH2:11][CH2:12][NH:13][CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[O:23][CH3:24])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 516892Sodium BicarbonateHCID 15380922HCID 15380922、化合物

生成物 1

HCID 15380923HCID 15380923、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒HCID 6344Dichloromethane溶媒

実験手順

A catalyst composed of palladium on 10% moist carbon (1.5 g) is added to a solution of N-cyclohexyl-5-[benzyl{2-(2-methoxyphenoxy)ethyl}amino]pentan-amide (3 g, 6.8 mmole) in glacial acetic acid (30 ml) and the mixture is hydrogenated for 2 hours at 20° C. The catalyst is removed by filtration and the solvent is evaporated under reduced pressure. The residue obtained in the form of a salt of acetic acid is taken up in dichloromethane (50 ml) and the base is liberated by treatment with a saturated solution of sodium hydrogen carbonate. The organic phase is collected, washed with water, dried over magnesium sulfate and the solvent is evaporated under reduced pressure. The expected product is obtained in the form of a white powder after crystallisation in diethylether (0.95 g, 40%).

後処理

  1. customThe catalyst is removed by filtration
  2. customthe solvent is evaporated under reduced pressure
  3. customThe residue obtained in the form of a salt of acetic acid
  4. customThe organic phase is collected
  5. washwashed with water
  6. dry with materialdried over magnesium sulfate
  7. customthe solvent is evaporated under reduced pressure

出典と根拠

ORDレコード
ord-29b105d75a934ead962d7185fd212f04
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998666

反応ノート

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