Ethylenediamine → HCID 86751684、化合物

HRID 1938151ノート

反応式

HRID 1938151 の反応式
[CH:1]([N:4]([CH2:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[O:30][CH3:31])[CH2:5][C:6]#[C:7][CH2:8][NH:9][C:10]([C:12]12[CH2:21][CH:16]3[CH2:17][CH:18]([CH2:20][CH:14]([CH2:15]3)[CH2:13]1)[CH2:19]2)=[O:11])([CH3:3])[CH3:2].C(N)CN.[BH4-].[Na+]>C(O)C.O.O.O.O.O.O.[Ni](Cl)Cl>[CH:1]([N:4]([CH2:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[O:30][CH3:31])[CH2:5][CH:6]=[CH:7][CH2:8][NH:9][C:10]([C:12]12[CH2:21][CH:16]3[CH2:15][CH:14]([CH2:20][CH:18]([CH2:17]3)[CH2:19]1)[CH2:13]2)=[O:11])([CH3:3])[CH3:2]

参加物

6

反応物 3

HCID 3301EthylenediamineHCID 4311764Sodium borohydrideHCID 86751685HCID 86751685、化合物

生成物 1

HCID 86751684HCID 86751684、化合物収率 79.6%

試薬・触媒・溶媒 2

HCID 11791229Dichloronickel;hexahydrate触媒HCID 702Ethanol溶媒

実験手順

A mixture of adamantane-1-carboxylic acid (4-{isopropyl-[2-(2-methoxyphenyl)ethyl]amino}but-2-ynyl)amide, (90 mg, 0.21 mmol), nickel chloride hexahydrate (60 mg, 0.25 mmol), ethylenediamine (0.15 ml, 0.25 mmol) and sodium borohydride (0.25 ml 1N solution in EtOH, 0.25 mmol) in 5 ml ethanol was stirred at ambient temperature for 10 h. The mixture was filtered, the solvent removed and the residue taken up in methylene chloride and washed with water. Evaporation of the solvent gave 71 mg of an oil.

後処理

  1. filtrationThe mixture was filtered
  2. customthe solvent removed
  3. washwashed with water
  4. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-cb410290233e46ce8da19ce652fc8d0d
出典データセット
uspto-grants-1997_12
特許番号
US05693630

反応ノート

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