Sodium borohydride → 3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-ol

HRID 274080ノート

反応式

HRID 274080 の反応式
[CH3:1][O:2][C:3]1[CH:14]=[CH:13][C:6]2[CH2:7][CH2:8][CH2:9][C:10](=[O:12])[CH2:11][C:5]=2[CH:4]=1.[BH4-].[Na+]>CO>[CH3:1][O:2][C:3]1[CH:14]=[CH:13][C:6]2[CH2:7][CH2:8][CH2:9][CH:10]([OH:12])[CH2:11][C:5]=2[CH:4]=1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 105595743-Methoxy-6,7,8,9-tetrahydro-5H-benzo[7]annulen-6-one

生成物 1

HCID 200947203-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-ol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-one (220 g) in methanol (1300 ml) was added portionwise sodium borohydride (22.0 g) at 6° C.-30° C., and then the reaction mixture was stirred for 40 minutes and evaporated in vacuo. The residue was partitioned between ethyl acetate (1 l) and water (1 l). The organic layer was washed with 1N hydrochloric acid (500 ml), aqueous sodium hydrogen carbonate (500 ml), and brine (200 ml), and dried over magnesium sulfate. The solvent was evaporated in vacuo to give 3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-ol as a white powder.

後処理

  1. customevaporated in vacuo
  2. customThe residue was partitioned between ethyl acetate (1 l) and water (1 l)
  3. washThe organic layer was washed with 1N hydrochloric acid (500 ml), aqueous sodium hydrogen carbonate (500 ml), and brine (200 ml)
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated in vacuo

出典と根拠

ORDレコード
ord-0361da08f81c4e1da779d4da0c028911
出典データセット
uspto-grants-1995_02
特許番号
US05387710

反応ノート

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