Thionyl Chloride → [3,4-bis(difluoromethoxy)phenyl]-(2-bromo-5-pyridyl) chloromethane

HRID 567953ノート

反応式

HRID 567953 の反応式
[F:1][CH:2]([F:23])[O:3][C:4]1[CH:5]=[C:6]([CH:14]([C:16]2[CH:17]=[N:18][C:19]([Br:22])=[CH:20][CH:21]=2)O)[CH:7]=[CH:8][C:9]=1[O:10][CH:11]([F:13])[F:12].O=S(Cl)[Cl:26].C([O-])(O)=O.[Na+]>C(Cl)Cl>[F:1][CH:2]([F:23])[O:3][C:4]1[CH:5]=[C:6]([CH:14]([C:16]2[CH:17]=[N:18][C:19]([Br:22])=[CH:20][CH:21]=2)[Cl:26])[CH:7]=[CH:8][C:9]=1[O:10][CH:11]([F:13])[F:12]

参加物

5

反応物 3

HCID 24386Thionyl ChlorideHCID 516892Sodium BicarbonateHCID 10971303HCID 10971303、化合物

生成物 1

HCID 11144147[3,4-bis(difluoromethoxy)phenyl]-(2-bromo-5-pyridyl) chloromethane

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution [3,4-Bis(difluoromethoxy)phenyl]-(6-bromo-3-pyridyl)methanol (15.8 g,40.0 mmol) in 400 mL of CH2Cl2, was added 3.8 mL (52.0 nimol) of SOCl2. The solution was stirred 45 minutes at room temperature and poured into a saturated aqueous solution of NaHCO3. The aqueous layer was extracted with CH2Cl2 and the combined organic layers were dry over MgSO4 and concentrated under reduced pressure. The crude chloride was used directly for the next step without any purification.

後処理

  1. extractionThe aqueous layer was extracted with CH2Cl2
  2. dry with materialthe combined organic layers were dry over MgSO4
  3. concentrationconcentrated under reduced pressure
  4. customThe crude chloride was used directly for the next step without any purification

出典と根拠

ORDレコード
ord-3bab9832e953440686340ca9eaff7b20
出典データセット
uspto-grants-2001_01
特許番号
US06180650B2

反応ノート

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