Triethylamine → HCID 86705165、化合物

HRID 2401259ノート

反応式

HRID 2401259 の反応式
C(N(CC)CC)C.C1(O[C:15](=[O:27])[NH:16][C:17]2[CH:18]=[N:19][C:20]([C:23]([F:26])([F:25])[F:24])=[CH:21][CH:22]=2)C=CC=CC=1.[NH2:28][C@H:29]([CH2:33][OH:34])[CH:30]([CH3:32])[CH3:31]>C(Cl)(Cl)Cl>[OH:34][CH2:33][C@@H:29]([NH:28][C:15]([NH:16][C:17]1[CH:18]=[N:19][C:20]([C:23]([F:24])([F:25])[F:26])=[CH:21][CH:22]=1)=[O:27])[CH:30]([CH3:32])[CH3:31]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 640993L-ValinolHCID 11173582Carbamic acid, [6-(trifluoromethyl)-3-pyridinyl]-, phenyl ester

生成物 1

HCID 86705165HCID 86705165、化合物収率 113.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
80 °C

実験手順

Triethylamine (0.54 mL) and phenyl[6-(trifluoromethyl)pyridin-3-yl]carbamate (600 mg) were added to a solution of L-valinol (200 mg) in chloroform, and the mixture was stirred at 80° C. for 1 hr. The reaction mixture was concentrated under reduced pressure, and the residue was purified by column chromatography (silica gel cartridge, hexane/ethyl acetate) to afford 1-[(2S)-1-hydroxy-3-methylbutan-2-yl]-3-[6-(trifluoromethyl)pyridin-3-yl]urea (640 mg).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was purified by column chromatography (silica gel cartridge, hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-5a51699867224141a54c18f102344ac8
出典データセット
uspto-grants-2014_08
特許番号
US08796272B2

反応ノート

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