Hydrochloric Acid → 3-Chloro-5-hydroxy-1-iodo-2-[3-(5-trifluoromethylpyrid-2-yloxy)propyloxy]-benzene

HRID 497052ノート

反応式

HRID 497052 の反応式
C([O:9][C:10]1[CH:11]=[C:12]([Cl:32])[C:13]([O:17][CH2:18][CH2:19][CH2:20][O:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][N:23]=2)=[C:14]([I:16])[CH:15]=1)(=O)C1C=CC=CC=1.[OH-].[Na+].Cl>O1CCCC1.CO>[Cl:32][C:12]1[C:13]([O:17][CH2:18][CH2:19][CH2:20][O:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:29])[F:30])=[CH:24][N:23]=2)=[C:14]([I:16])[CH:15]=[C:10]([OH:9])[CH:11]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 223186095-Benzoyloxy-3-chloro-1-iodo-2-[3-(5-trifluoromethylpyrid-2-yloxy)propyloxy]benzene

生成物 1

HCID 223186173-Chloro-5-hydroxy-1-iodo-2-[3-(5-trifluoromethylpyrid-2-yloxy)propyloxy]-benzene

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

3.12 g of 5-benzoyloxy-3-chloro-1-iodo-2-[3-(5-trifluoromethylpyrid-2-yloxy)propyloxy]benzene were dissolved in 16 ml of tetrahydrofuran and 7.8 ml of methanol, and 3.9 ml of 2N aqueous sodium hydroxide solution were added. After 30 minutes of stirring at room temperature. 3.9 ml of 2N hydrochloric acid were added, and the reaction mixture was concentrated under reduced pressure. Saturated sodium chloride solution and ethyl acetate were added to the residue, and the mixture was shaken. The ethyl acetate phase was isolated, dried and concentrated. The resulting crude product was purified chromatographically. Yield: 2.03 g (80%)

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. additionSaturated sodium chloride solution and ethyl acetate were added to the residue
  3. stirringthe mixture was shaken
  4. customThe ethyl acetate phase was isolated
  5. customdried
  6. concentrationconcentrated
  7. customThe resulting crude product was purified chromatographically

出典と根拠

ORDレコード
ord-0b1f00f0866c4f468d1216b30b5bd9f7
出典データセット
uspto-grants-2005_09
特許番号
US06949551B2

反応ノート

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