Sodium Hydroxide → HCID 53929886、化合物

HRID 274082ノート

反応式

HRID 274082 の反応式
C([O:4][C@@H:5]1[CH2:11][CH2:10][CH2:9][C:8]2[CH:12]=[CH:13][C:14]([O:16][CH3:17])=[CH:15][C:7]=2[CH2:6]1)(=O)C.[OH-].[Na+]>CO.O>[CH3:17][O:16][C:14]1[CH:13]=[CH:12][C:8]2[CH2:9][CH2:10][CH2:11][C@@H:5]([OH:4])[CH2:6][C:7]=2[CH:15]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 53866555HCID 53866555、化合物

生成物 1

HCID 53929886HCID 53929886、化合物収率 97.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of (R)-3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl acetate (136 g) in methanol (1.36 l) was added dropwise a solution of sodium hydroxide (46.4 g) in water (232 ml) at ambient temperature. The reaction mixture was stirred for 1 hour and evaporated in vacuo. The residue was partitioned between ethyl acetate (1.1 l) and brine (550 ml). The organic layer was washed with 1N hydrochloric acid solution (550 ml), 1N aqueous sodium hydroxide solution (550 ml), and brine (550 ml), dried over magnesium sulfate, and evaporated in vacuo to give (R)-3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-ol (108.96 g) as a white powder.

後処理

  1. customevaporated in vacuo
  2. customThe residue was partitioned between ethyl acetate (1.1 l) and brine (550 ml)
  3. washThe organic layer was washed with 1N hydrochloric acid solution (550 ml), 1N aqueous sodium hydroxide solution (550 ml), and brine (550 ml)
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-3c6f7a1f01b6413a98dd619ea1b16fd8
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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