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Butyl bromide → 4-amino-N-[(4-benzyl-2-morpholinyl)methyl]-2-butoxy-5-chlorobenzamide

HRID 1608203
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HRID 1608203 반응식
[NH2:1][C:2]1[C:24]([Cl:25])=[CH:23][C:5]([C:6]([NH:8][CH2:9][CH:10]2[O:15][CH2:14][CH2:13][N:12]([CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH2:11]2)=[O:7])=[C:4]([OH:26])[CH:3]=1.[CH2:27](Br)[CH2:28][CH2:29][CH3:30]>[OH-].[Na+].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.ClCCl>[NH2:1][C:2]1[C:24]([Cl:25])=[CH:23][C:5]([C:6]([NH:8][CH2:9][CH:10]2[O:15][CH2:14][CH2:13][N:12]([CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH2:11]2)=[O:7])=[C:4]([O:26][CH2:27][CH2:28][CH2:29][CH3:30])[CH:3]=1
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참가 물질

6

반응물 2

HCID 8002Butyl bromideHCID 148819784-amino-N-[(4-benzyl-2-morpholinyl)methyl]-5-chloro-2-hydroxybenzamide

생성물 1

HCID 148819104-amino-N-[(4-benzyl-2-morpholinyl)methyl]-2-butoxy-5-chlorobenzamide수율 119.6%

시약·촉매·용매 3

HCID 74236Tetrabutylammonium Bromide촉매HCID 6344Dichloromethane용매
HCID 14798
Sodium Hydroxide
용매

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온도
25 °C

실험 절차

To a stirred solution of 4-amino-N-[(4-benzyl-2-morpholinyl)methyl]-5-chloro-2-hydroxybenzamide (4.0 g) in 1N aqueous sodium hydroxide solution (32 ml), tetrabutylammonium bromide (3.4 g) and a solution of butyl bromide (4.3 g) in dichloromethane (32 ml) are added. The reaction mixture is stirred at 25° C. for 15 hours and concentrated under reduced pressure. To the residue is added ethyl acetate. The organic layer is washed successively with water and saturated aqueous sodium chloride solution, dried over magnesium sulfate, and evaporated under reduced pressure. The residue is chromatographed on silica gel with methanol-chloroform (5:95) to give the title compound (5.5 g) as an oil. The free base thus obtained is dissolved in hot ethanol (20 ml), and fumaric acid (1.5 g) is added. The solution is stirred for some time. The precipitate is collected and recrystallized from ethanol to give the fumarate hemihydrate (4.6 g) of the title compound, mp 188°-190° C.

후처리

  1. concentrationconcentrated under reduced pressure
  2. additionTo the residue is added ethyl acetate
  3. washThe organic layer is washed successively with water and saturated aqueous sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure
  6. customThe residue is chromatographed on silica gel with methanol-chloroform (5:95)

출처 및 근거

ORD 기록
ord-97fe459743bc434899e871f1528483df
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04870074

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