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4-Chlorobutyryl chloride → 1-(6-Acetyl-4-chloro-3'-fluoro-3-methylbiphenyl-2-yl)pyrrolidin-2-one

HRID 510834
ノート
印刷プレビュー

反応式

HRID 510834 の反応式
[NH2:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([F:14])[CH:9]=2)=[C:6]([C:15](=[O:17])[CH3:16])[CH:5]=[C:4]([Cl:18])[C:3]=1[CH3:19].Cl[CH2:21][CH2:22][CH2:23][C:24](Cl)=[O:25].CC(C)([O-])C.[K+]>CN(C)C1C=CN=CC=1.O1CCCC1>[C:15]([C:6]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([F:14])[CH:9]=2)=[C:2]([N:1]2[CH2:21][CH2:22][CH2:23][C:24]2=[O:25])[C:3]([CH3:19])=[C:4]([Cl:18])[CH:5]=1)(=[O:17])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 783704-Chlorobutyryl chlorideHCID 23665647Potassium tert-butoxideHCID 583684301-(6-Amino-4-chloro-3'-fluoro-5-methylbiphenyl-2-yl)ethanone

生成物 1

HCID 866667671-(6-Acetyl-4-chloro-3'-fluoro-3-methylbiphenyl-2-yl)pyrrolidin-2-one収率 30%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒
HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

To a mixture of 1-(6-amino-4-chloro-3′-fluoro-5-methylbiphenyl-2-yl)ethanone (100 mg, 0.4 mmol) and 4-dimethylaminopyridine (52.8 mg, 0.432 mmol) in tetrahydrofuran (1 mL) was added 4-chlorobutanoyl chloride (0.044 mL, 0.40 mmol). The reaction was stirred at room temperature for 1 hour. Potassium tert-butoxide (1.0 M) in tetrahydrofuran (0.79 mL, 0.79 mmol) was added and the resulting mixture was stirred at room temperature for 2 hours, then quenched with aq. ammonium chloride and extracted with ethyl acetate. The combined organic layers were washed with water, brine, dried and evaporated. The resulting residue was purified on silica gel, eluting with 0 to 50% ethyl acetate in hexane, to give the product (40 mg, 30%). LCMS calculated for C19H18ClFNO2 (M+H)+: m/z=346.1. found: 346.1.

後処理

  1. stirringthe resulting mixture was stirred at room temperature for 2 hours
  2. customquenched with aq. ammonium chloride
  3. extractionextracted with ethyl acetate
  4. washThe combined organic layers were washed with water, brine
  5. customdried
  6. customevaporated
  7. customThe resulting residue was purified on silica gel
  8. washeluting with 0 to 50% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-e8fdab7e8e4d4477ab95268edd4ecead
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096600B2

反応ノート

読み込み中…

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