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

HRID 566118노트

반응식

HRID 566118 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
50 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-4b29fc6e59aa4adaa5910712f7dc454c
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06172061B2

반응 노트

불러오는 중…