Propranolol Hydrochloride → HCID 53833412, 화합물

HRID 845723

반응식

HRID 845723 반응식
[CH3:1][CH:2]([NH:4][CH2:5][CH:6]([OH:19])[CH2:7][O:8][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=[CH:11][CH:10]=1)[CH3:3].Cl.CN(C1C2C(N(C)C)=CC=CC=2C=CC=1)C.Cl[C:38]([O:40][CH:41]([Cl:43])[CH3:42])=[O:39]>C(Cl)(Cl)Cl>[Cl:43][CH:41]([O:40][C:38]([N:4]([CH:2]([CH3:1])[CH3:3])[CH2:5][CH:6]([OH:19])[CH2:7][O:8][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=[CH:11][CH:10]=1)=[O:39])[CH3:42]

참가 물질

5

반응물 3

HCID 62882Propranolol HydrochlorideHCID 88675Proton spongeHCID 5213051-Chloroethyl chloroformate

생성물 1

HCID 53833412HCID 53833412, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A suspension of propanolol hydrochloride (3.0 g) in chloroform (100 ml) was mixed with proton sponge® (4.3 g) and cooled in an ice bath. 1-Chloroethyl chloroformate (1.5 g) was added dropwise to the reaction mixture. The suspension dissolved in about 5 minutes. The cooling bath was removed and the reaction mixture was stirred at room temperature for 1.5 hours. The chloroform solution was washed with water, 3N HCl and water successively. The organic layer was dried over Na2SO4 and evaporated to a thick oil weighing 3.6 g. NMR (CDCl3) δ1.25 (6H, d, J=7 Hz, CH(Me)2), 1.8 (3H, d, J=7 Hz, CH3CH), 3.3=3.6 (3H, m, ArOCH2 and CH(Me)2), 4.0-4.6 (3H, m, NCH2 and CHOH), 6.61 (1H, q, J=7 Hz, CH3CH) and 6.7-8.4 (7H, m, aromatic). IR (film) ν3450, 1715, 1583, 1270, 1248, 1108 cm-1.

후처리

  1. temperaturecooled in an ice bath
  2. dissolutionThe suspension dissolved in about 5 minutes
  3. customThe cooling bath was removed
  4. washThe chloroform solution was washed with water, 3N HCl and water successively
  5. dry with materialThe organic layer was dried over Na2SO4
  6. customevaporated to a thick oil

출처 및 근거

ORD 기록
ord-7dc69a75ea4c464c9a630191f4f46948
출처 데이터셋
uspto-grants-1988_07
특허 번호
US04760057

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