Ammonium Chloride → HCID 178447899、化合物

HRID 1245269

反応式

HRID 1245269 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1Br.[Mg].[CH2:11]([C@H:14]1[CH2:19][CH2:18][C@H:17]([CH:20]2[CH2:25][CH2:24][C:23](=[O:26])[CH2:22][CH2:21]2)[CH2:16][CH2:15]1)[CH2:12][CH3:13].[Cl-].[NH4+]>C1COCC1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[C:23]1([OH:26])[CH2:22][CH2:21][CH:20]([C@H:17]2[CH2:18][CH2:19][C@H:14]([CH2:11][CH2:12][CH3:13])[CH2:15][CH2:16]2)[CH2:25][CH2:24]1

参加物

6

反応物 4

HCID 25517Ammonium ChlorideHCID 678622-Bromo-1,4-difluorobenzeneHCID 5462224MagnesiumHCID 178447904HCID 178447904、化合物

生成物 1

HCID 178447899HCID 178447899、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
50 °C

実験手順

A solution of 2,5-difluorobromobenzene (1.33 mmol) in THF (10 ml) is added dropwise to magnesium (1.44 mmol). After the addition is completed, the reaction mixture is stirred at 50° C. for 2 hrs. To the reaction mixture, a solution of 4-(trans-4-propylcyclohexyl)cyclohexanone (1.03 mmol) in THF (10 ml) is added dropwise. After the addition is completed, the reaction mixture is stirred for 2 hrs at 50° C. A saturated aqueous solution of ammonium chloride (10 ml) is added in small portions and the aqueous layer is extracted with ethyl acetate (100 ml) twice. The extract is washed with water, and then dried over anhydrous magnesium sulfate. The titled compound is obtained by evaporation of the solvent under reduced pressure.

後処理

  1. additionAfter the addition
  2. additionAfter the addition
  3. stirringthe reaction mixture is stirred for 2 hrs at 50° C
  4. extractionthe aqueous layer is extracted with ethyl acetate (100 ml) twice
  5. washThe extract is washed with water
  6. dry with materialdried over anhydrous magnesium sulfate

出典と根拠

ORDレコード
ord-becb4e41da5b4a20ad9f930593b35783
出典データセット
uspto-grants-2006_10
特許番号
US07125589B1

関連ノート

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