2-{4-[4-(3,4-dichlorophenoxy)piperidin-1-yl]-3-hydroxybutyl}-1H-isoindole-1,3(2H)-dione → 4-Amino-1-[4-(3,4-dichlorophenoxy)piperidin-1-yl]butan-2-ol

HRID 2233369ノート

反応式

HRID 2233369 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:28]=[CH:29][C:30]=1[Cl:31])[O:5][CH:6]1[CH2:11][CH2:10][N:9]([CH2:12][CH:13]([OH:27])[CH2:14][CH2:15][N:16]2C(=O)C3C(=CC=CC=3)C2=O)[CH2:8][CH2:7]1>C(O)C.NN>[NH2:16][CH2:15][CH2:14][CH:13]([OH:27])[CH2:12][N:9]1[CH2:8][CH2:7][CH:6]([O:5][C:4]2[CH:28]=[CH:29][C:30]([Cl:31])=[C:2]([Cl:1])[CH:3]=2)[CH2:11][CH2:10]1

参加物

4

反応物 1

HCID 592960492-{4-[4-(3,4-dichlorophenoxy)piperidin-1-yl]-3-hydroxybutyl}-1H-isoindole-1,3(2H)-dione

生成物 1

HCID 592960694-Amino-1-[4-(3,4-dichlorophenoxy)piperidin-1-yl]butan-2-ol収率 97.3%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 9321Hydrazine溶媒

実験手順

A solution of mixture of 2-{4-[4-(3,4-dichlorophenoxy)piperidin-1-yl]-3-hydroxybutyl}-1H-isoindole-1,3(2H)-dione (3.00 g) in a mixture of ethanol (75 ml) and 35% aqueous hydrazine (15 ml) was heated at reflux 4 h. The mixture was cooled down and the solvents removed under vacuum. The residue was triturated with warm dichloromethane. The white solid was removed by filtration and the filtrate dried over sodium sulfate. The mixture was filtered and the solvent was evaporated to afford the title compound as a yellow oil (2.10 g) which was used without further purification in the next step.

後処理

  1. temperaturewas heated
  2. temperatureat reflux 4 h
  3. temperatureThe mixture was cooled down
  4. customthe solvents removed under vacuum
  5. customThe residue was triturated with warm dichloromethane
  6. customThe white solid was removed by filtration
  7. dry with materialthe filtrate dried over sodium sulfate
  8. filtrationThe mixture was filtered
  9. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-428c9bd6d8d746a9a58888bb410875e8
出典データセット
uspto-grants-2010_05
特許番号
US07709500B2

反応ノート

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