Hydrochloric Acid → Verapamil

HRID 2414989

反応式

HRID 2414989 の反応式
[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]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 62969Verapamil Hydrochloride

生成物 1

HCID 2520Verapamil

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 24602Deuterium Oxide溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c59805b31aca4d7084c4f0a7006741c0
出典データセット
uspto-grants-2004_11
特許番号
US06818200B2

関連ノート

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