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

HRID 1006242ノート

反応式

HRID 1006242 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
40 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-8b25129524f4496a848ee70643f1c89c
出典データセット
uspto-grants-2004_09
特許番号
US06787653B2

反応ノート

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