Potassium Carbonate → HCID 59190377、化合物

HRID 219625

反応式

HRID 219625 の反応式
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

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 852999(alphaS)-4-Bromo-alpha-methylbenzenemethanamineHCID 59190391HCID 59190391、化合物

生成物 1

HCID 59190377HCID 59190377、化合物収率 30.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-866cf1e4c35044579d28f1e177a45e92
出典データセット
uspto-grants-2012_06
特許番号
US08202857B2

関連ノート

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