Ethyl isocyanate → HCID 69818250、化合物

HRID 2417421ノート

反応式

HRID 2417421 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C@H:9]([N:12]([CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH2:13][C@H:14]([OH:23])[CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:10][OH:11])=[CH:4][CH:3]=1.[CH2:31]([N:33]=[C:34]=[O:35])[CH3:32]>ClCCl>[CH2:24]([N:12]([C@H:9]([CH2:10][OH:11])[CH2:8][C:5]1[CH:6]=[CH:7][C:2]([NH:1][C:34]([NH:33][CH2:31][CH3:32])=[O:35])=[CH:3][CH:4]=1)[CH2:13][C@H:14]([OH:23])[CH2:15][O:16][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1)[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1

参加物

4

反応物 2

HCID 8022Ethyl isocyanateHCID 69817666HCID 69817666、化合物

生成物 1

HCID 69818250HCID 69818250、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To an ice-cooled solution of (2S)-3-(4-aminophenyl)-2-[N-benzyl-N-[(2S)-2-hydroxy-3-phenoxypropyl]amino]-1-propanol (83 mg) in dichloromethane (0.8 ml) was added dropwise ethyl isocyanate (0.016 ml). The mixture was stirred at the same temperature for 1.5 hours and partitioned between chloroform and saturated sodium bicarbonate solution. The organic layer was separated, washed with brine, dried over magnesium sulfate, and filtered. The filtrate was concentrated and the residue was purified by column chromatography (silica gel, chloroform/methanol) to give N-[4-[(2S)-2-[N-benzyl-N-[(2S)-2-hydroxy-3-phenoxypropyl]amino]-3-hydroxypropyl]phenyl]-N′-ethylurea (84 mg) as a white amorphous powder.

後処理

  1. custompartitioned between chloroform and saturated sodium bicarbonate solution
  2. customThe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated
  7. customthe residue was purified by column chromatography (silica gel, chloroform/methanol)

出典と根拠

ORDレコード
ord-0b4fcbea45e64776ac8f193f0cad535e
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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