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

HRID 1277293노트

반응식

HRID 1277293 반응식
C[N:2]1[NH:6][N:5]=[C:4]([C:7]2[CH:8]=[CH:9][C:10]3[O:16][CH2:15][CH2:14][C:13]([C:17]([O:19]C)=[O:18])=[CH:12][C:11]=3[CH:21]=2)[NH:3]1.[OH-].[Na+].Cl.[CH3:25]O>C1COCC1>[CH3:25][N:3]1[C:4]([C:7]2[CH:8]=[CH:9][C:10]3[O:16][CH2:15][CH2:14][C:13]([C:17]([OH:19])=[O:18])=[CH:12][C:11]=3[CH:21]=2)=[N:5][N:6]=[N:2]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 18472406methyl 7-(2-methyl-1H-tetrazol-5-yl)-2,3-dihydro-1-benzoxepine-4-carboxylate

생성물 1

HCID 184726577-(1-methyl-1H-tetrazol-5-yl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid수율 95%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

In methanol (3 ml) and THF (3 ml) was dissolved methyl 7-(2-methyl-1H-tetrazol-5-yl)-2,3-dihydro-1-benzoxepine-4-carboxylate (76 mg, 0.27 mmol), and to the mixture was added 1N sodium hydroxide solution (0.8 ml). The mixture was stirred at 50° C. for 4 hours, and to the mixture was added, under ice-cooling, 1N hydrochloric acid (0.8 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-(1-methyl-1H-tetrazol-5-yl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid (69 mg, 0.25 mmol, 95%).

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-20878c647361461f92c2d435430ba42d
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06166006

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