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Hydrochloric Acid → HCID 19423990、化合物

HRID 743227
ノート
印刷プレビュー

反応式

HRID 743227 の反応式
[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]
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 313Hydrochloric AcidHCID 7922Succinic anhydrideHCID 107612473-Dimethylamino-1-[2-(4-phenylbutyl)phenoxy]-2-propanol

生成物 1

HCID 19423990HCID 19423990、化合物収率 93%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bf99c4e7ee674c179990be667d99555e
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05556864

反応ノート

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