Water → HCID 67371748、化合物

HRID 1436122ノート

反応式

HRID 1436122 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[F:7][C:8]1[CH:9]=[C:10]([C@H:16]2[NH:21][C@@H:20]([C:22](OC)=[O:23])[CH2:19][CH2:18][CH2:17]2)[CH:11]=[C:12]([F:15])[C:13]=1[F:14].O.[OH-].[Na+]>C1COCC1>[F:15][C:12]1[CH:11]=[C:10]([C@H:16]2[NH:21][C@@H:20]([CH2:22][OH:23])[CH2:19][CH2:18][CH2:17]2)[CH:9]=[C:8]([F:7])[C:13]=1[F:14]

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 67372196methyl (2R,6S)-6-(3,4,5-trifluorophenyl)piperidine-2-carboxylate

生成物 1

HCID 67371748HCID 67371748、化合物収率 99.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-20 °C

実験手順

LAH (75 mg) was added in three portions to a solution of methyl(2R,6S)-6-(3,4,5-trifluorophenyl)piperidine-2-carboxylate (270 mg) in THF (5 mL) at −20° C. over 15 minutes. The reaction solution was stirred at −20° C. for one hour, and water (0.1 mL), a 5 N sodium hydroxide solution (0.1 mL), and water (0.3 mL) were sequentially added to the reaction solution. The mixture was heated to room temperature and filtered through celite. The filtrate was concentrated under reduced pressure to obtain 242 mg of the title compound. The property value of the compound is as follows.

後処理

  1. temperatureThe mixture was heated to room temperature
  2. filtrationfiltered through celite
  3. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-d655c5d48b754930a4b237930493c662
出典データセット
uspto-grants-2009_11
特許番号
US07618960B2

反応ノート

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