Dichloromethane → HCID 59843359, 화합물

HRID 253046노트

반응식

HRID 253046 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([CH2:14]O)=[C:12]([CH:16]([CH3:18])[CH3:17])[N:11]=[C:10]([S:19][CH3:20])[N:9]=2)=[CH:4][CH:3]=1.ClCCl.P(Br)(Br)[Br:25]>O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([CH2:14][Br:25])=[C:12]([CH:16]([CH3:18])[CH3:17])[N:11]=[C:10]([S:19][CH3:20])[N:9]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 24614Phosphorus tribromideHCID 29980411[4-(4-Fluorophenyl)-2-(methylsulfanyl)-6-(propan-2-yl)pyrimidin-5-yl]methanol2회

생성물 1

HCID 59843359HCID 59843359, 화합물수율 90.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

14.6 g (50 mmol) of compound (9) and 200 ml of dichloromethane were added into a 500 mL three-neck round bottomed flask, equipped with a mechanical stirrer and a dropping funnel, followed by addition of 67 g (0.1 mol) of phosphorus tribromide dropwise at room temperature. After TLC assay showed that the starting compound (9) was depleted, 100 mL of water was added, and the organic layer was collected. The organic phase was then washed with 5% aqueous NaHCO3 solution, dried over anhydrous calcium chloride, and evaporated under reduced pressure to remove the solvent, obtaining 16 g raw product of compound (7), which was used directly in the next step without purification.

후처리

  1. customequipped with a mechanical stirrer and a dropping funnel
  2. customthe organic layer was collected
  3. washThe organic phase was then washed with 5% aqueous NaHCO3 solution
  4. dry with materialdried over anhydrous calcium chloride
  5. customevaporated under reduced pressure
  6. customto remove the solvent

출처 및 근거

ORD 기록
ord-70b6a49d0cbf47f19d2a0598113920bc
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07872012B2

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