Anisole → HCID 10340129、化合物

HRID 370658

反応式

HRID 370658 の反応式
C([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=[O:36])[CH2:16][N:17]2[CH2:22][CH2:21][N:20]([CH:23]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH2:19][CH2:18]2)=[CH:11][CH:10]=1)C1C=CC=CC=1.C1(OC)C=CC=CC=1>C(O)(=O)C.Br>[C:30]1([CH:23]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[N:20]2[CH2:19][CH2:18][N:17]([CH2:16][C:15]([C:12]3[CH:11]=[CH:10][C:9]([OH:8])=[CH:14][CH:13]=3)=[O:36])[CH2:22][CH2:21]2)[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1

参加物

5

反応物 2

HCID 7519AnisoleHCID 103227601-(4-Benzyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanone

生成物 1

HCID 10340129HCID 10340129、化合物収率 62%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 260Hydrogen Bromide溶媒

実験手順

12.5 g (26 mmol) of 1-(4-benzyloxyphenyl)-2-(4-diphenylmethyl-piperazinyl)ethanone and 2.8 g (26 mmol) of anisole were dissolved in a mixture of 37.5 ml of acetic acid and 12.5 ml of 47% hydrobromic acid. The resultant mixture was heated to reflux for 1 hour. After being cooled to room temperautre, the reaction mixture was washed with 200 ml of ether and then with 50 ml of ether to remove acetic acid. The resultant solution was neutralized with an aqueous 2N solution of sodium hydroxide. Separated organic substances were extracted with 120 ml of ethyl acetate and then washed with saturated saline. The ethyl acetate solution was dried over anhydrous sodium sulfate and then concentrated. The residue was taken up in 60 ml of isopropanol and allowed to stand at room temperature to give 6.28 g of crude crystals of 2-(4-diphenylmethylpiperazinyl)-1-(4-hydroxyphenyl)ethanone (yield: 62%).

後処理

  1. temperatureto reflux for 1 hour
  2. temperatureAfter being cooled to room temperautre
  3. washthe reaction mixture was washed with 200 ml of ether
  4. customwith 50 ml of ether to remove acetic acid
  5. extractionSeparated organic substances were extracted with 120 ml of ethyl acetate
  6. washwashed with saturated saline
  7. dry with materialThe ethyl acetate solution was dried over anhydrous sodium sulfate
  8. concentrationconcentrated
  9. customto stand at room temperature

出典と根拠

ORDレコード
ord-ff844af5aea943b1b43f1a93ac133f60
出典データセット
uspto-grants-1985_07
特許番号
US04528194

関連ノート

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