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

HRID 274080노트

반응식

HRID 274080 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0361da08f81c4e1da779d4da0c028911
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05387710

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