N-[2-(4-benzyloxycarbonylamino-1-piperidinyl)ethyl]-1-(2-propyl)-1H-indazole-3-carboxamide oxalate → N-[2-(4-amino-1-piperidinyl)ethyl]-1-(2-propyl)-1H-indazole-3-carboxamide dioxalate

HRID 399051ノート

反応式

HRID 399051 の反応式
[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].C(OC([NH:17][CH:18]1[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][NH:26][C:27]([C:29]2[C:37]3[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=3)[N:31]([CH:38]([CH3:40])[CH3:39])[N:30]=2)=[O:28])[CH2:20][CH2:19]1)=O)C1C=CC=CC=1.[H][H]>[Pd].C(O)C>[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].[NH2:17][CH:18]1[CH2:19][CH2:20][N:21]([CH2:24][CH2:25][NH:26][C:27]([C:29]2[C:37]3[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=3)[N:31]([CH:38]([CH3:40])[CH3:39])[N:30]=2)=[O:28])[CH2:22][CH2:23]1

参加物

5

反応物 2

HCID 18969263N-[2-(4-benzyloxycarbonylamino-1-piperidinyl)ethyl]-1-(2-propyl)-1H-indazole-3-carboxamide oxalateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 86751129N-[2-(4-amino-1-piperidinyl)ethyl]-1-(2-propyl)-1H-indazole-3-carboxamide dioxalate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

The product from Example 8, as the free base (8.71 g, 18.8 mmol), was reacted with hydrogen gas in the presence of 5% Pd/C (25° C./18 h/60 PSI) in an ethanol solution. After filtering the catalyst, the ethanol was evaporated to 5.0 g oil. Crystallization as the dioxalate salt from methanol/water provided colorless crystals. Mp 232° C. Mass spectrum, m+ =329. Anal (C22H31N5O9) theory C, 51.86; H, 6.13; N, 13.75; found C, 51.61; H, 6.04; N, 13.48.

後処理

  1. filtrationAfter filtering the catalyst
  2. customthe ethanol was evaporated to 5.0 g oil
  3. customCrystallization as the dioxalate salt from methanol/water provided colorless crystals

出典と根拠

ORDレコード
ord-13e870af2be645bf8f4ef154ba77eb5f
出典データセット
uspto-grants-1998_10
特許番号
US05817676

反応ノート

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