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Oxalyl chloride → (E)-1-[4-(4-ethoxy-6-methyl-2-pyridyl)piperazin-1-yl]-4,4,4-trifluoro-but-2-en-1-one

HRID 1775377
ノート
印刷プレビュー

反応式

HRID 1775377 の反応式
[F:1][C:2]([F:9])([F:8])/[CH:3]=[CH:4]/[C:5](O)=[O:6].C(Cl)(=O)C(Cl)=O.Cl.[CH2:17]([O:19][C:20]1[CH:25]=[C:24]([CH3:26])[N:23]=[C:22]([N:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)[CH:21]=1)[CH3:18]>ClCCl.CN(C=O)C.C(OCC)(=O)C>[CH2:17]([O:19][C:20]1[CH:25]=[C:24]([CH3:26])[N:23]=[C:22]([N:27]2[CH2:28][CH2:29][N:30]([C:5](=[O:6])/[CH:4]=[CH:3]/[C:2]([F:9])([F:8])[F:1])[CH2:31][CH2:32]2)[CH:21]=1)[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 65578Oxalyl chlorideHCID 57096144,4,4-Trifluorocrotonic acidHCID 898258231-(4-Ethoxy-6-methyl-2-pyridyl)piperazine hydrochloride

生成物 1

HCID 89826076(E)-1-[4-(4-ethoxy-6-methyl-2-pyridyl)piperazin-1-yl]-4,4,4-trifluoro-but-2-en-1-one収率 41%

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒
HCID 6344
Dichloromethane
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

(E)-4,4,4-Trifluorobut-2-enoic acid (17 mg, 0.12 mmol) was dissolved in dichloromethane (1 ml), oxalyl chloride (11 μl, 0.12 mmol) was added and the resulting solution was stirred at room temperature for 10 minutes. This solution was added to a solution of 1-(4-ethoxy-6-methyl-2-pyridyl)piperazine hydrochloride (22 mg, 0.086 mmol) and TEA (42 μl, 0.3 mmol) in anhydrous DMF (0.5 ml) and the resulting mixture was stirred at room temperature for one hour. The mixture was diluted with ethyl acetate, washed with sat. sodium bicarbonate solution, brine, dried (magnesium sulfate) and concentrated under reduced pressure. The residue was purified by preparative HPLC (Waters X-Bridge, gradient of water containing 0.1% NH3 and acetonitrile) to yield 12 mg of a solid (0.035 mmol, yield 41%).

後処理

  1. stirringthe resulting mixture was stirred at room temperature for one hour
  2. washwashed with sat. sodium bicarbonate solution, brine
  3. dry with materialdried (magnesium sulfate)
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by preparative HPLC (Waters X-Bridge, gradient of water containing 0.1% NH3 and acetonitrile)

出典と根拠

ORDレコード
ord-d2618898ff9b4635860a96f4e08d4b49
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09260441B2

反応ノート

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