HCID 10165245、化合物 → HCID 10185014、化合物

HRID 854362ノート

反応式

HRID 854362 の反応式
[C:1]([C:5]1[CH:36]=[CH:35][C:8]([C:9]([N:11]2[C@@H:15]([C:16]3[S:20][C:19](Cl)=[N:18][CH:17]=3)[C@@H:14]([C:22]3[CH:27]=[N:26][CH:25]=[CH:24][N:23]=3)[CH2:13][C@@:12]2([CH2:31][CH:32]([CH3:34])[CH3:33])[C:28]([OH:30])=[O:29])=[O:10])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2]>[Pd].C(O)C>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([C:9]([N:11]2[C@@H:15]([C:16]3[S:20][CH:19]=[N:18][CH:17]=3)[C@@H:14]([C:22]3[CH:27]=[N:26][CH:25]=[CH:24][N:23]=3)[CH2:13][C@@:12]2([CH2:31][CH:32]([CH3:33])[CH3:34])[C:28]([OH:30])=[O:29])=[O:10])=[CH:35][CH:36]=1)([CH3:3])([CH3:2])[CH3:4]

参加物

4

反応物 1

HCID 10165245HCID 10165245、化合物

生成物 1

HCID 10185014HCID 10185014、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A mixture of Example 27 (40 mg, 0.076 mmol) and 10% palladium on carbon catalyst (40 mg) in ethanol (5 mL) was hydrogenated over 5 days. The catalyst was removed by filtration and washed with ethanol. Following evaporation of the solvent the title compound was purified by reverse phase HPLC on a C18 column using a two-solvent gradient elution with (A) water containing formic acid (0.1%) and (B) acetonitrile-water (95:5 v/v) containing formic acid (0.05%) as the eluents, and analysis of the fractions by electrospray mass spectroscopy.

後処理

  1. customThe catalyst was removed by filtration
  2. washwashed with ethanol
  3. customevaporation of the solvent the title compound
  4. customwas purified by reverse phase HPLC on a C18 column
  5. washa two-solvent gradient elution with (A) water
  6. additioncontaining formic acid (0.1%) and (B) acetonitrile-water (95:5 v/v)
  7. additioncontaining formic acid (0.05%) as the eluents, and analysis of the fractions by electrospray mass spectroscopy

出典と根拠

ORDレコード
ord-4c159ad349394425b2bc428a27ac2463
出典データセット
uspto-grants-2007_08
特許番号
US07259163B2

反応ノート

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