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Hydrochloric Acid → HCID 19423990, 화합물

HRID 743227
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HRID 743227 반응식
[C:1]1(=[O:7])[O:6][C:4](=[O:5])[CH2:3][CH2:2]1.[CH3:8][N:9]([CH3:31])[CH2:10][CH:11]([OH:30])[CH2:12][O:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH2:20][CH2:21][CH2:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[ClH:32]>CC(C)=O.O1CCOCC1>[ClH:32].[C:4]([O:30][CH:11]([CH2:12][O:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH2:20][CH2:21][CH2:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[CH2:10][N:9]([CH3:8])[CH3:31])(=[O:5])[CH2:3][CH2:2][C:1]([OH:6])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 7922Succinic anhydrideHCID 107612473-Dimethylamino-1-[2-(4-phenylbutyl)phenoxy]-2-propanol

생성물 1

HCID 19423990HCID 19423990, 화합물수율 93%

시약·촉매·용매 2

HCID 180Acetone용매HCID 312751,4-Dioxane용매

실험 절차

0.57 g of succinic anhydride was added to a solution of 1.79 g of 3-dimethylamino-1-[2-(4-phenylbutyl)phenoxy]-2-propanol [prepared as described in Example 1(b)] in 50 ml of acetone, and the resulting mixture was heated under reflux for 2 hours. At the end of this time, the reaction mixture was cooled, and 1.5 ml of a 4N solution of hydrogen chloride in dioxane were added, and the mixture was allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 2.20 g (yield 93%) of the title compound as colorless crystals, melting at 123°-125° C.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 2 hours
  3. temperatureAt the end of this time, the reaction mixture was cooled
  4. customto stand at room temperature
  5. customThe crystals which precipitated
  6. filtrationwere collected by filtration
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-bf99c4e7ee674c179990be667d99555e
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05556864

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