Hydrochloric Acid → 7-(2-methyl-1H-tetrazol-5-yl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid

HRID 566118ノート

反応式

HRID 566118 の反応式
C1COCC1.[CH3:6][N:7]1[NH:11][N:10]=[C:9]([C:12]2[CH:13]=[CH:14][C:15]3[O:21][CH2:20][CH2:19][C:18]([C:22]([O:24]C)=[O:23])=[CH:17][C:16]=3[CH:26]=2)[NH:8]1.[OH-].[Na+].Cl>CO>[CH3:6][N:7]1[NH:11][N:10]=[C:9]([C:12]2[CH:13]=[CH:14][C:15]3[O:21][CH2:20][CH2:19][C:18]([C:22]([OH:24])=[O:23])=[CH:17][C:16]=3[CH:26]=2)[NH:8]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 18472406methyl 7-(2-methyl-1H-tetrazol-5-yl)-2,3-dihydro-1-benzoxepine-4-carboxylate

生成物 1

HCID 184724317-(2-methyl-1H-tetrazol-5-yl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid収率 96%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

In methanol (7 ml) and THF (7 ml) was suspended methyl 7-(2-methyl-1H-tetrazol-5-yl)-2,3-dihydro-1-benzoxepine-4-carboxylate (324 mg, 1.13 mmol), and to the mixture was added 1N sodium hydroxide solution (3.4 ml). The mixture was stirred at 50° C. for 4 hours, and to the mixture was added, under ice-cooling, 1N hydrochloric acid(3.4 ml). The mixture was concentrated under reduced pressure, and to the residue was added water. Insoluble materials were filtered, which were washed with water and dried under reduced pressure to give 7-(2-methyl-1H-tetrazol-5-yl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid (295 mg, 1.08 mmol, 96%).

後処理

  1. additionto the mixture was added, under ice-
  2. temperaturecooling
  3. concentrationThe mixture was concentrated under reduced pressure
  4. additionto the residue was added water
  5. filtrationInsoluble materials were filtered
  6. washwhich were washed with water
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-4b29fc6e59aa4adaa5910712f7dc454c
出典データセット
uspto-grants-2001_01
特許番号
US06172061B2

反応ノート

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