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Ammonium Chloride → 2,2-Difluorocyclopropyl(4-chlorophenyl) ketone

HRID 561449
ノート
印刷プレビュー

反応式

HRID 561449 の反応式
[F:1][C:2]1([F:11])[CH2:4][CH:3]1[C:5](N(OC)C)=[O:6].Cl[Mg][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[Br-].[Cl-:21].[NH4+]>C1COCC1.C(OCC)C>[Cl:21][C:14]1[CH:19]=[CH:18][C:17]([C:5]([CH:3]2[CH2:4][C:2]2([F:11])[F:1])=[O:6])=[CH:16][CH:15]=1
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 25517Ammonium ChlorideHCID 534161312,2-difluoro-N-methoxy-N-methylcyclopropane-1-carboxamideHCID 178419578HCID 178419578、化合物

生成物 1

HCID 248658712,2-Difluorocyclopropyl(4-chlorophenyl) ketone

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran
溶媒
2 回

実験手順

A solution of 2.00 g (12.1 mmol) of the compound from Example 120A in 20 ml of THF was added under argon to 2.87 g (13.3 mmol) of a 1N chlorophenylmagnesium bromide solution in diethyl ether in 20 ml of THF at RT, and the mixture was heated under reflux for 2 h. The reaction mixture was added to saturated aqueous ammonium chloride solution and extracted twice with diethyl ether, and the combined organic phases were dried over magnesium sulfate and concentrated. 2.47 g (94% of theory) of the title compound were obtained and were reacted without further purification.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 h
  3. extractionextracted twice with diethyl ether
  4. dry with materialthe combined organic phases were dried over magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-2dc7db6623e64040b431f836187bbf19
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08063234B2

反応ノート

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