Potassium Carbonate → HCID 59190377, 화합물

HRID 219625

반응식

HRID 219625 반응식
BrC1C=CC([C@@H](N)C)=CC=1.[Br:11][C:12]1[CH:17]=[CH:16][C:15]([C@@H:18]([N:20]2[CH2:26][CH2:25][CH2:24][C:23]([CH2:33][C:34]([CH3:36])=[CH2:35])([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[O:22]C2=O)[CH3:19])=[CH:14][CH:13]=1.C([O-])([O-])=O.[K+].[K+]>CC#N>[Br:11][C:12]1[CH:13]=[CH:14][C:15]([C@@H:18]([NH:20][CH2:26][CH2:25][CH2:24][C:23]([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)([OH:22])[CH2:33][C:34]([CH3:36])=[CH2:35])[CH3:19])=[CH:16][CH:17]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 852999(alphaS)-4-Bromo-alpha-methylbenzenemethanamineHCID 59190391HCID 59190391, 화합물

생성물 1

HCID 59190377HCID 59190377, 화합물수율 30.4%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of (S)-1-(4-bromo-phenyl)-ethyl amine (3.58 g, 0.018 mol) in dry CH3CN (350 mL) was added 3-((1S)-1-(4-bromophenyl)ethyl)-7-(2-methylallyl)-7-phenyl-1,3-oxazepan-2-one (4.2 g, 0.018 mol), KI (3.19 g, 0.019 mol), and K2CO3 (3.73 g, 0.027 mol). The mixture was stirred at reflux overnight, filtered, and concentrated to give the crude product, which was purified by column chromatography to give 7-((1S)-1-(4-bromophenyl)ethylamino)-2-methyl-4-phenylhept-1-en-4-ol (2.2 g, 30%) as an oil.

후처리

  1. temperatureat reflux overnight
  2. filtrationfiltered
  3. concentrationconcentrated
  4. customto give the crude product, which
  5. customwas purified by column chromatography

출처 및 근거

ORD 기록
ord-866cf1e4c35044579d28f1e177a45e92
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202857B2

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