Methanol → HCID 59557735、化合物

HRID 425042ノート

反応式

HRID 425042 の反応式
C([O:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][C:13]2[CH:18]=[C:17]([Br:19])[CH:16]=[CH:15][C:14]=2[Cl:20])=[CH:8][CH:7]=1)(=O)C.C1COCC1.CO.O[Li].O>C(OCC)(=O)C.O>[Br:19][C:17]1[CH:16]=[CH:15][C:14]([Cl:20])=[C:13]([CH:18]=1)[CH2:12][C:9]1[CH:10]=[CH:11][C:6]([CH2:5][OH:4])=[CH:7][CH:8]=1

参加物

7

反応物 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 59557783HCID 59557783、化合物

生成物 1

HCID 59557735HCID 59557735、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 4-(5-bromo-2-chlorobenzyl)benzyl acetate (intermediate AJ) (8.86 g) in 60 mL of a mixture of THF:MeOH:H2O (v/v/v=2:3:1), LiOH.H2O (2.10 g) was added. The solution was stirred at room temperature. After 1 h, H2O (10 mL) and ethyl acetate (100 mL) were added. The aqueous layer was extracted 2× with ethyl acetate. The combined ethyl acetate layers were washed with brine and dried over Na2SO4. The solvent was evaporated under reduced pressure, and the product was purified by column chromatography to obtain pure intermediate AK (6 g).

後処理

  1. extractionThe aqueous layer was extracted 2× with ethyl acetate
  2. washThe combined ethyl acetate layers were washed with brine
  3. dry with materialdried over Na2SO4
  4. customThe solvent was evaporated under reduced pressure
  5. customthe product was purified by column chromatography
  6. customto obtain pure intermediate AK (6 g)

出典と根拠

ORDレコード
ord-c1fc6659a0c346719e908427ab79420a
出典データセット
uspto-grants-2012_01
特許番号
US08106021B2

反応ノート

読み込み中…