Water → HCID 84045984、化合物

HRID 625697

反応式

HRID 625697 の反応式
[Br:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[CH:4][C:3]=1[CH2:10][CH2:11][C:12]([O:14]C)=[O:13].O>[OH-].[Na+].CC(O)C>[Br:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[CH:4][C:3]=1[CH2:10][CH2:11][C:12]([OH:14])=[O:13]

参加物

5

実験手順

Methyl 3-(2-bromo-3,5-difluorophenyl)propanoate (prepared as described in Step 1, 4.3 g) in aqueous NaOH (4 M, 13.5 mL) and 2-propanol (30 mL) is heated at 50° C. for 2 hours. Water is added, the mixture washed with diethyl ether, acidified to ca. pH 5 by adding concentrated aqueous HCl, and extracted twice with diethyl ether. The combined extracts of the acidified mixture are washed with brine and volatiles evaporated under reduced pressure. The resulting material (Yield 3.6 g) is used in the next step without further purification. LC (METHOD 7): tR=0.99 min.

後処理

  1. washthe mixture washed with diethyl ether
  2. additionby adding concentrated aqueous HCl
  3. extractionextracted twice with diethyl ether
  4. washThe combined extracts of the acidified mixture are washed with brine and volatiles
  5. customevaporated under reduced pressure
  6. customThe resulting material (Yield 3.6 g) is used in the next step without further purification

出典と根拠

ORDレコード
ord-c0c3a2f4b8794fad9273437e85495432
出典データセット
uspto-grants-2016_04
特許番号
US09308194B2

関連ノート

読み込み中…