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 2233369노트

반응식

HRID 2233369 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 9321Hydrazine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-428c9bd6d8d746a9a58888bb410875e8
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709500B2

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