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Pyridine → 1-(6,7-Dimethoxy-1,2,3,4-tetrahydroisoquinolin-2-yl)-3-methyl-2-bromobutan-1-one

HRID 1760042
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HRID 1760042 반응식
[Br:1][CH:2]([CH:6]([CH3:8])[CH3:7])[C:3](Cl)=[O:4].N1C=CC=CC=1.Cl.[CH3:16][O:17][C:18]1[CH:19]=[C:20]2[C:25](=[CH:26][C:27]=1[O:28][CH3:29])[CH2:24][NH:23][CH2:22][CH2:21]2>CN(C1C=CN=CC=1)C.C(Cl)(Cl)Cl>[CH3:16][O:17][C:18]1[CH:19]=[C:20]2[C:25](=[CH:26][C:27]=1[O:28][CH3:29])[CH2:24][N:23]([C:3](=[O:4])[CH:2]([Br:1])[CH:6]([CH3:8])[CH3:7])[CH2:22][CH2:21]2
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참가 물질

6

반응물 3

HCID 1049PyridineHCID 64560356,7-Dimethoxy-1,2,3,4-tetrahydroisoquinoline hydrochlorideHCID 124869822-Bromo-3-methylbutanoyl chloride

생성물 1

HCID 225999051-(6,7-Dimethoxy-1,2,3,4-tetrahydroisoquinolin-2-yl)-3-methyl-2-bromobutan-1-one

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매
HCID 6212
Chloroform
용매

실험 절차

Racemic body α-bromoisovaleryl chloride (327 mg, 1.64 mmol) on the market and 4-(N,N-dimethylamino)pyridine (about 10 mg) were added to a pyridine (8 ml) suspension of 6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline hydrochloride (472 mg, 2.05 mmol), and the mixture was stirred at room temperature for 3 hours. The reaction solution was diluted with chloroform (50 ml), washed with 1 N hydrochloric acid (50 ml) and a 1 N aqueous sodium hydroxide solution (50 ml), dried over anhydrous magnesium sulfate, concentrated under reduced pressure, and used, without isolating and purifying the obtained gummy substance, in the reactions in Examples 27 and 28.

후처리

  1. washwashed with 1 N hydrochloric acid (50 ml)
  2. dry with materiala 1 N aqueous sodium hydroxide solution (50 ml), dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customwithout isolating
  5. custompurifying the obtained gummy substance

출처 및 근거

ORD 기록
ord-6e76426ace1e4384a81ea634dd877b6e
출처 데이터셋
uspto-grants-2005_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06838465B2

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