Acetic Acid → HCID 22329126、化合物

HRID 586843ノート

反応式

HRID 586843 の反応式
[C:1](O)(=[O:3])C.C(O)=O.[CH2:8]([O:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[CH:21]=[CH:22][C:23]3[NH:29][CH2:28][CH2:27][C:26]([C:30]([O:32][CH3:33])=[O:31])=[CH:25][C:24]=3[CH:34]=2)=[CH:16][CH:15]=1)[CH3:9]>C1COCC1>[CH2:8]([O:10][CH2:11][CH2:12][O:13][C:14]1[CH:15]=[CH:16][C:17]([C:20]2[CH:21]=[CH:22][C:23]3[N:29]([CH:1]=[O:3])[CH2:28][CH2:27][C:26]([C:30]([O:32][CH3:33])=[O:31])=[CH:25][C:24]=3[CH:34]=2)=[CH:18][CH:19]=1)[CH3:9]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 284Formic AcidHCID 22329032methyl 7-[4-(2-ethoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate

生成物 1

HCID 22329126HCID 22329126、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
50 °C

実験手順

To anhydrous acetic acid (0.25 ml) was added formic acid (0.13 ml) under ice-cooling, and the mixture was stirred under nitrogen atmosphere at 50° C. for 2 hours. To the mixture was added THF (2 ml) and then was added dropwise, under ice-cooling, a solution of methyl 7-[4-(2-ethoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate (0.25 g) in THF (10 ml), and the mixture was stirred at room temperature overnight. The solvent was evaporated, and to the residue was added water. The mixture was extracted with ethyl acetate. The organic layer was washed with sodium hydrogen carbonate solution, water and saturated brine, and dried with anhydrous magnesium sulfate, and the solvent was evaporated to give methyl 7-[4-(2-ethoxyethoxy)phenyl]-1-formyl-2,3-dihydro-1H-1-benzazepine-4-carboxylate (0.2 g) as colorless crystals.

後処理

  1. temperaturecooling
  2. additionwas added dropwise, under ice-
  3. temperaturecooling
  4. customThe solvent was evaporated
  5. additionto the residue was added water
  6. extractionThe mixture was extracted with ethyl acetate
  7. washThe organic layer was washed with sodium hydrogen carbonate solution, water and saturated brine
  8. dry with materialdried with anhydrous magnesium sulfate
  9. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-ddac9a40c8724e6ea2d022ac0aa74ab6
出典データセット
uspto-grants-2005_08
特許番号
US06936602B1

反応ノート

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