HCID 10165245, 화합물 → HCID 10185014, 화합물

HRID 854362노트

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HRID 854362 반응식
[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]

참가 물질

4

반응물 1

HCID 10165245HCID 10165245, 화합물

생성물 1

HCID 10185014HCID 10185014, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4c159ad349394425b2bc428a27ac2463
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07259163B2

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