Ammonium Chloride → HCID 178447899, 화합물

HRID 1245269

반응식

HRID 1245269 반응식
[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

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 678622-Bromo-1,4-difluorobenzeneHCID 5462224MagnesiumHCID 178447904HCID 178447904, 화합물

생성물 1

HCID 178447899HCID 178447899, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-becb4e41da5b4a20ad9f930593b35783
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07125589B1

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