1-(1-Naphthyl)piperazine → 6-(2-(4-(1-Naphthyl)-piperazinyl)ethyl)benzothiazolone

HRID 365372

反応式

HRID 365372 の反応式
Br[CH2:2][CH2:3][C:4]1[CH:13]=[CH:12][C:7]2[N:8]=[CH:9][S:10](=[O:11])[C:6]=2[CH:5]=1.[C:14]1([N:24]2[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]2)[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:17]=[CH:16][CH:15]=1.C(=O)([O-])[O-].[Na+].[Na+]>CC(CC(C)C)=O>[C:14]1([N:24]2[CH2:29][CH2:28][N:27]([CH2:2][CH2:3][C:4]3[CH:13]=[CH:12][C:7]4[N:8]=[CH:9][S:10](=[O:11])[C:6]=4[CH:5]=3)[CH2:26][CH2:25]2)[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:17]=[CH:16][CH:15]=1

参加物

5

反応物 3

HCID 13421-(1-Naphthyl)piperazineHCID 10340Sodium CarbonateHCID 692279736-(2-Bromoethyl)benzothiazolone

生成物 1

HCID 692310686-(2-(4-(1-Naphthyl)-piperazinyl)ethyl)benzothiazolone

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

To a 100 ml round-bottomed flask with condenser and nitrogen inlet were added 1.0 gram (3.88 mmol) of 6-(2-bromoethyl)benzothiazolone, 822 mg (3.88 mmol) N-(1-naphthyl)piperazine, 410 mg (3.88 mmol) sodium carbonate, and 50 ml methylisobutlyketone. The reaction was refluxed for 24 hours, cooled, and evaporated. The residue was taken up in ethyl acetate, washed with water and brine, dried over sodium sulfate, and evaporated. The resulting solid was treated with hot ethyl acetate to afford a white solid, m.p. 198°-220° C., 540 mg (36%).

後処理

  1. temperatureThe reaction was refluxed for 24 hours
  2. temperaturecooled
  3. customevaporated
  4. washwashed with water and brine
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. additionThe resulting solid was treated with hot ethyl acetate
  8. customto afford a white solid, m.p. 198°-220° C., 540 mg (36%)

出典と根拠

ORDレコード
ord-423c04872b3a492c8470d3dbbe872319
出典データセット
uspto-grants-2000_10
特許番号
US06127373

関連ノート

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