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Tetrahydrofuran → HCID 9841264, 화합물

HRID 1032948
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HRID 1032948 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][O:23][CH3:24])=[C:17]([N:25]([CH3:27])[CH3:26])[CH:16]=2)[O:9][CH2:10][CH2:11][N:12]([CH3:14])[CH3:13])=[CH:4][CH:3]=1.O1CCCC1.C(=O)([O-])O.[Na+]>Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][O:23][CH3:24])=[C:17]([N:25]([CH3:26])[CH3:27])[CH:16]=2)[OH:9])=[CH:6][CH:7]=1.[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:15]2[CH:20]=[CH:19][C:18]([OH:21])=[C:17]([N:25]([CH3:27])[CH3:26])[CH:16]=2)[O:9][CH2:10][CH2:11][N:12]([CH3:14])[CH3:13])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8028TetrahydrofuranHCID 516892Sodium BicarbonateHCID 190269862-[1-(4-chlorophenyl)-1-(3-dimethylamino-4-methoxymethoxyphenyl)methoxy]-N,N-dimethylethanamine

생성물 2

HCID 9841264HCID 9841264, 화합물HCID 190269591-(4-Chlorophenyl)-1-(3-dimethylamino-4-methoxymethoxyphenyl)methanol

시약·촉매·용매 1

HCID 313
Hydrochloric Acid
용매
2회

실험 절차

A solution of the compound (2) (0.43 g, 1.09 mmol) obtained above in 1N hydrochloric acid (3.28 ml) and tetrahydrofuran (2 ml) was heated under reflux for 3 hours. Thereto was added additional 1N hydrochloric acid (2.18 ml) and the mixture was further heated for 1.5 hours. The reaction mixture was poured into a saturated aqueous solution of sodium hydrogencarbonate, extracted with methylene chloride, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by column chromatography on silica gel to give the title compound (Compound 1). Yield 0.15 g (39%).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. temperaturethe mixture was further heated for 1.5 hours
  4. extractionextracted with methylene chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated
  7. customThe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-9338b6e3b521439b98db916fc2cc591e
출처 데이터셋
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05308840

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