Hydrochloric Acid → 2-chloro-4-(methylsulfonyl)-N-(1-(2-methoxyethyl)tetrazol-5-yl)-benzamide

HRID 68215노트

반응식

HRID 68215 반응식
[Cl:1][C:2]1[CH:10]=[C:9]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[NH2:15][C:16]1[N:20]([CH2:21][CH2:22][O:23][CH3:24])[N:19]=[N:18][N:17]=1.O.Cl>N1C=CC=CC=1.CC(=O)OCC>[Cl:1][C:2]1[CH:10]=[C:9]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([NH:15][C:16]1[N:20]([CH2:21][CH2:22][O:23][CH3:24])[N:19]=[N:18][N:17]=1)=[O:5]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 11128804Benzoyl chloride, 2-chloro-4-(methylsulfonyl)-HCID 583353441-(2-methoxyethyl)-1H-1,2,3,4-tetrazol-5-amine

생성물 1

HCID 867235572-chloro-4-(methylsulfonyl)-N-(1-(2-methoxyethyl)tetrazol-5-yl)-benzamide

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 8857Ethyl Acetate용매

반응 조건

온도
60 °C

실험 절차

176 mg (0.75 mmol) of 2-chloro-4-(methylsulfonyl)benzoyl chloride, 145 mg (1.0 mmol) of 5-amino-1-(2-methoxyethyl)tetrazole in 2 ml of pyridine are stirred at 60° C. for 12 h. 0.1 ml of water is then added, the mixture is stirred at 60° C. for 30 min and EA and 2N HCl are added. The organic phase is separated off and washed with 2N HCl and brine, dried over Na2SO4, concentrated and purified by RP—HPLC (acetonitrile/water). Yield 66 mg (23%).

후처리

  1. customThe organic phase is separated off
  2. washwashed with 2N HCl and brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. custompurified by RP—HPLC (acetonitrile/water)

출처 및 근거

ORD 기록
ord-c8af9790b4d94610883b5f1185ffa93e
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822378B2

반응 노트

불러오는 중…