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

HRID 249162노트

반응식

HRID 249162 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7cd6604b53ae436bae4087f1e89d673a
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05212320

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