Hydrochloric Acid → Verapamil

HRID 1456876

반응식

HRID 1456876 반응식
[CH3:1][CH:2]([C:4]([C:24]1[CH:25]=[CH:26][C:27]([O:32][CH3:33])=[C:28]([O:30][CH3:31])[CH:29]=1)([C:22]#[N:23])[CH2:5][CH2:6][CH2:7][N:8]([CH2:10][CH2:11][C:12]1[CH:13]=[CH:14][C:15]([O:20][CH3:21])=[C:16]([O:18][CH3:19])[CH:17]=1)[CH3:9])[CH3:3].Cl.Cl>[2H]O[2H].CCOCC>[CH3:3][CH:2]([C:4]([C:24]1[CH:25]=[CH:26][C:27]([O:32][CH3:33])=[C:28]([O:30][CH3:31])[CH:29]=1)([C:22]#[N:23])[CH2:5][CH2:6][CH2:7][N:8]([CH2:10][CH2:11][C:12]1[CH:13]=[CH:14][C:15]([O:20][CH3:21])=[C:16]([O:18][CH3:19])[CH:17]=1)[CH3:9])[CH3:1]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 62969Verapamil Hydrochloride

생성물 1

HCID 2520Verapamil

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 24602Deuterium Oxide용매

반응 조건

온도
90 °C

실험 절차

Verapamil hydrochloride was added to a solution of 25% deuterated sulfuric acid in deuterated water (v/v) and deuterated methanol. The solution was stirred for 140 hours at 90° C. The pH was adjusted to 12.0 and the mixture extracted with ethyl acetate. The combined ethyl acetate extracts were washed with water, dried over magnesium sulfate and evaporated to yield a viscous oil. This oil was dissolved in ether and ethereal hydrochloride was added to precipitate the hydrochloride salt. The salt was collected by filtration and crystallized from ethyl acetate to obtain deuterated verapamil as a white solid.

후처리

  1. extractionthe mixture extracted with ethyl acetate
  2. washThe combined ethyl acetate extracts were washed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. customto yield a viscous oil
  6. customto precipitate the hydrochloride salt
  7. filtrationThe salt was collected by filtration
  8. customcrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-ccb7ca7648b54acba23ed3a73cb71f88
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05846514

연결된 노트

불러오는 중…