Hydrochloric Acid → 1,3-Bis[4-[4-(3,5-dimethoxy-4-propoxyphenyl) benzoyl)-1-piperazinyl]propane dihydrochloride

HRID 1006242노트

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HRID 1006242 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:15]2[CH:59]=[CH:58][C:18]([C:19]([N:21]3[CH2:26][CH2:25][N:24]([CH2:27][CH2:28][CH2:29][N:30]4[CH2:35][CH2:34][N:33]([C:36](=[O:57])[C:37]5[CH:42]=[CH:41][C:40]([C:43]6[CH:48]=[C:47]([O:49][CH3:50])[C:46]([O:51][CH2:52][CH2:53][CH3:54])=[C:45]([O:55][CH3:56])[CH:44]=6)=[CH:39][CH:38]=5)[CH2:32][CH2:31]4)[CH2:23][CH2:22]3)=[O:20])=[CH:17][CH:16]=2)[CH:6]=[C:7]([O:13][CH3:14])[C:8]=1[O:9][CH2:10][CH2:11][CH3:12].C(OCC)(=O)C.[ClH:66].C(OCC)C>CO>[ClH:66].[ClH:66].[CH3:50][O:49][C:47]1[CH:48]=[C:43]([C:40]2[CH:39]=[CH:38][C:37]([C:36]([N:33]3[CH2:34][CH2:35][N:30]([CH2:29][CH2:28][CH2:27][N:24]4[CH2:25][CH2:26][N:21]([C:19](=[O:20])[C:18]5[CH:58]=[CH:59][C:15]([C:5]6[CH:4]=[C:3]([O:2][CH3:1])[C:8]([O:9][CH2:10][CH2:11][CH3:12])=[C:7]([O:13][CH3:14])[CH:6]=6)=[CH:16][CH:17]=5)[CH2:22][CH2:23]4)[CH2:31][CH2:32]3)=[O:57])=[CH:42][CH:41]=2)[CH:44]=[C:45]([O:55][CH3:56])[C:46]=1[O:51][CH2:52][CH2:53][CH3:54]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 8857Ethyl AcetateHCID 102599621,3-Bis[4-[4-(3,5-dimethoxy-4-propoxyphenyl) benzoyl]-1-piperazinyl]propane

생성물 1

HCID 226768651,3-Bis[4-[4-(3,5-dimethoxy-4-propoxyphenyl) benzoyl)-1-piperazinyl]propane dihydrochloride수율 86%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
40 °C

실험 절차

To a solution of 4.2 g (5.19 mmol) of 1,3-bis[4-[4-(3,5-dimethoxy-4-propoxyphenyl) benzoyl]-1-piperazinyl]propane in methanol (30 mL) stirred in an ice bath, was added 3.2 mL (13 mmol) of a 4.0 mol/L ethyl acetate solution of hydrogen chloride, and the mixture was concentrated under reduced pressure. Methanol (50 mL) was added and the mixture was concentrated under reduced pressure again. A suspension of the residue in methanol-chloroform (10:1, 44 mL) was stirred at 40° C. to give a homogeneous solution. Diethyl ether (10 mL) was added to the solution and the mixture was stirred at room temperature and at 0° C. Precipitates were collected by filtration and washed successively with methanol-diethyl ether (2:3) and diethyl ether to afford 3.92 g of 1,3-bis[4-[4-(3,5-dimethoxy-4-propoxyphenyl) benzoyl)-1-piperazinyl]propane dihydrochloride as a colorless crystalline powder (yield: 86%).

후처리

  1. concentrationthe mixture was concentrated under reduced pressure
  2. additionMethanol (50 mL) was added
  3. concentrationthe mixture was concentrated under reduced pressure again
  4. additionA suspension of the residue in methanol-chloroform (10:1, 44 mL)
  5. customto give a homogeneous solution
  6. stirringthe mixture was stirred at room temperature and at 0° C
  7. customPrecipitates
  8. filtrationwere collected by filtration
  9. washwashed successively with methanol-diethyl ether (2:3) and diethyl ether

출처 및 근거

ORD 기록
ord-8b25129524f4496a848ee70643f1c89c
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06787653B2

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