Sodium Hydroxide → 3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-ylmethyl)benzoic acid

HRID 249162ノート

反応式

HRID 249162 の反応式
[OH-].[Na+].[CH:3]1[C:13]2[CH2:12][CH2:11][C:10]3[CH:14]=[CH:15][CH:16]=[CH:17][C:9]=3[N:8]([CH2:18][C:19]3[CH:20]=[C:21]([CH:26]=[CH:27][CH:28]=3)[C:22]([O:24]C)=[O:23])[C:7]=2[CH:6]=[CH:5][CH:4]=1>O1CCOCC1.CO>[CH:14]1[C:10]2[CH2:11][CH2:12][C:13]3[CH:3]=[CH:4][CH:5]=[CH:6][C:7]=3[N:8]([CH2:18][C:19]3[CH:20]=[C:21]([CH:26]=[CH:27][CH:28]=3)[C:22]([OH:24])=[O:23])[C:9]=2[CH:17]=[CH:16][CH:15]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 19024806methyl 3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-ylmethyl)benzoate

生成物 1

HCID 190248733-(10,11-dihydro-5H-dibenz[b,f]azepin-5-ylmethyl)benzoic acid収率 99.3%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
25 °C

実験手順

1N aqueous solution of sodium hydroxide (9 ml) was added to a solution of methyl 3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-ylmethyl)benzoate (1.06 g) in a mixture of 1,4-dioxane (25 ml) and methanol (15 ml) at 25° C. The mixture was stirred at 25° C. for 3 hours, and then at 50° C. for 30 minutes. After evaporation of the solvent, the residue was partitioned between ethyl acetate and 0.1N hydrochloric acid. The organic layer was separated, washed with water and brine, dried over magnesium sulfate, and evaporated to give 3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-ylmethyl)benzoic acid (1.01 g) as powder.

後処理

  1. waitat 50° C. for 30 minutes
  2. customAfter evaporation of the solvent
  3. customthe residue was partitioned between ethyl acetate and 0.1N hydrochloric acid
  4. customThe organic layer was separated
  5. washwashed with water and brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated

出典と根拠

ORDレコード
ord-7cd6604b53ae436bae4087f1e89d673a
出典データセット
uspto-grants-1993_05
特許番号
US05212320

反応ノート

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