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Sodium Hydroxide → Pemafibrate

HRID 1712175
ノート
印刷プレビュー

反応式

HRID 1712175 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]([CH2:23][C:24]1[CH:25]=[C:26]([CH:41]=[CH:42][CH:43]=1)[O:27][C@H:28]([CH2:39][CH3:40])[C:29]([O:31]CC1C=CC=CC=1)=[O:30])[CH2:11][CH2:12][CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=1.[OH-].[Na+]>C(O)C>[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]([CH2:23][C:24]1[CH:25]=[C:26]([CH:41]=[CH:42][CH:43]=1)[O:27][C@H:28]([CH2:39][CH3:40])[C:29]([OH:31])=[O:30])[CH2:11][CH2:12][CH2:13][O:14][C:15]1[CH:16]=[CH:17][C:18]([O:21][CH3:22])=[CH:19][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 11856279benzyl (R)-2-[3-[N-(benzoxazol-2-yl)-N-(3-(4-methoxyphenoxy)propyl)aminomethyl]phenoxy]butyrate

生成物 1

HCID 11526038Pemafibrate収率 100.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Benzyl (R)-2-[3-[N-(benzoxazol-2-yl)-N-(3-(4-methoxyphenoxy)propyl)aminomethyl]phenoxy]butyrate (72 mg) was dissolved in ethanol (3 mL), and a 4 N aqueous sodium hydroxide solution (0.5 mL) was added at 0° C. Then, the resulting mixture was stirred at room temperature for 1 hour. The reaction liquor was concentrated under reduced pressure, and then was dissolved in chloroform (30 mL). The solution was washed with a saturated aqueous solution of ammonium chloride and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by preparative TLC (chloroform/methanol=10/1) to obtain a colorless solid (61 mg, 100%).

後処理

  1. concentrationThe reaction liquor was concentrated under reduced pressure
  2. dissolutionwas dissolved in chloroform (30 mL)
  3. washThe solution was washed with a saturated aqueous solution of ammonium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationAfter filtration
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customthe residue was purified by preparative TLC (chloroform/methanol=10/1)

出典と根拠

ORDレコード
ord-37f4e4f616f5467692da97ccb024f245
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07790903B2

反応ノート

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