HCID 69818250、化合物 → HCID 69818475、化合物

HRID 2417422ノート

反応式

HRID 2417422 の反応式
C([N:8]([C@H:20]([CH2:34][OH:35])[CH2:21][C:22]1[CH:27]=[CH:26][C:25]([NH:28][C:29]([NH:31][CH2:32][CH3:33])=[O:30])=[CH:24][CH:23]=1)[CH2:9][C@H:10]([OH:19])[CH2:11][O:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)C1C=CC=CC=1>CO.[Pd]>[CH2:32]([NH:31][C:29]([NH:28][C:25]1[CH:24]=[CH:23][C:22]([CH2:21][C@H:20]([NH:8][CH2:9][C@H:10]([OH:19])[CH2:11][O:12][C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH2:34][OH:35])=[CH:27][CH:26]=1)=[O:30])[CH3:33]

参加物

4

反応物 1

HCID 69818250HCID 69818250、化合物

生成物 1

HCID 69818475HCID 69818475、化合物収率 64.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of N-[4-[(2S)-2-[N-benzyl-N-[(2S)-2-hydroxy-3-phenoxypropyl]amino]-3-hydroxypropyl]phenyl]-N′-ethylurea (73 mg) in methanol (1.5 ml) was hydrogenated (1 atm) over 10% palladium on carbon (11 mg) at room temperature for 12 hours. After the catalyst was filtered off, the filtrate was concentrated and the residue was purified by column chromatography (silica gel, chloroform/methanol) followed by recrystallization from ehtanol/hexane to give N-ethyl-N′-[4-[(2S)-3-hydroxy-2-[[(2S)-2-hydroxy-3-phenoxypropyl]amino]-propyl]phenyl]urea (38 mg) as a white powder.

後処理

  1. customat room temperature
  2. customfor 12 hours
  3. filtrationAfter the catalyst was filtered off
  4. concentrationthe filtrate was concentrated
  5. customthe residue was purified by column chromatography (silica gel, chloroform/methanol)
  6. customfollowed by recrystallization from ehtanol/hexane

出典と根拠

ORDレコード
ord-f1aac32679234d3f9e962dbd6cba462a
出典データセット
uspto-grants-2004_11
特許番号
US06826033B2

反応ノート

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