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Tetrahydrofuran → HCID 9841264、化合物

HRID 1032948
ノート
印刷プレビュー

反応式

HRID 1032948 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 2

HCID 9841264HCID 9841264、化合物HCID 190269591-(4-Chlorophenyl)-1-(3-dimethylamino-4-methoxymethoxyphenyl)methanol

試薬・触媒・溶媒 1

HCID 313
Hydrochloric Acid
溶媒
2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-9338b6e3b521439b98db916fc2cc591e
出典データセット
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05308840

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート