Hydrochloric Acid → RS 93007

HRID 65308

반응식

HRID 65308 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([CH:32]([CH3:34])[CH3:33])([C:30]#[N:31])[CH2:12][CH2:13][CH2:14][CH:15]2[CH2:24][C:23]3[C:18](=[CH:19][C:20]([O:27][CH3:28])=[C:21]([O:25][CH3:26])[CH:22]=3)[CH2:17][N:16]2[CH3:29])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[ClH:35].CCOCC>C(O)(C)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([CH:32]([CH3:34])[CH3:33])([C:30]#[N:31])[CH2:12][CH2:13][CH2:14][CH:15]2[CH2:24][C:23]3[C:18](=[CH:19][C:20]([O:27][CH3:28])=[C:21]([O:25][CH3:26])[CH:22]=3)[CH2:17][N:16]2[CH3:29])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[ClH:35]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 1291023-(4-Cyano-4-(3,4-dimethoxyphenyl)-5-methylhex-1-yl)-1,2,3,4-tetrahydro-6,7-dimethoxy-2-methylisoquinoline

생성물 1

HCID 129101RS 93007

시약·촉매·용매 1

HCID 3776Isopropanol용매2회

실험 절차

The free base, 3-[4-(3,4-dimethoxyphenyl)-4-isopropyl-4-cyanobutyl]-6,7-dimethoxy-N-methyl-1,2,3,4-tetrahydroisoquinoline (1, 15 g, 0.032 mol) was dissolved in isopropanol (70 mL) at 70° C., and 6M HCl in isopropanol (5.6 mL) slowly added. After cooling to room temperature, ether (40 mL) was added until the solution became cloudy (saturated), and the resulting mixture stirred overnight. The resulting solid was collected, washed thoroughly with ether-isopropanol (1:1, 50 mL), and dried in vacuo at 50° C. to yield 3-[4-(3,4-dimethoxyphenyl)-4-isopropyl-4-cyanobutyl]-6,7-dimethoxy-N-methyl-1,2,3,4-tetrahydroisoquinoline·HCl (1·HCl, 13.7 g, m.p. 115°-120° C.) as a white powder.

후처리

  1. customThe resulting solid was collected
  2. washwashed thoroughly with ether-isopropanol (1:1, 50 mL)
  3. customdried in vacuo at 50° C.

출처 및 근거

ORD 기록
ord-f7b0d798c79c4e5d88ee89341c0c7a36
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04613606

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