Dimethylamine → 1-Butanamine, 4-(2-(2-(2-chlorophenyl)ethyl)phenoxy)-N,N-dimethyl-, hydrochloride

HRID 2285537ノート

反応式

HRID 2285537 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH2:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[Cl:21].[CH3:22][NH:23][CH3:24]>O1CCCC1>[ClH:21].[CH3:22][N:23]([CH3:24])[CH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH2:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[Cl:21]

参加物

4

反応物 2

HCID 674DimethylamineHCID 205450052-(4-Bromobutoxy)-2'-chlorobibenzyl

生成物 1

HCID 30553461-Butanamine, 4-(2-(2-(2-chlorophenyl)ethyl)phenoxy)-N,N-dimethyl-, hydrochloride収率 93%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 3.0 g of 2-(4-bromobutoxy)-2'-chlorobibenzyl in 15 ml of 50% aqueous dimethylamine solution and 15 ml of tetrahydrofuran was stirred at room temperature for 5 hours. The reaction mixture was concentrated and to the concentrate was added 2 N-NaOH solution. The product was extracted with ether, washed well with saturated sodium chloride solution and then dried over anhydrous sodium sulfate. To the ether solution was added 20% ethanolic hydrogen chloride to yield white crystals. Recrystallization from ethanol-ether gave 2.8 g (93% yield) of 2-(4-dimethylaminobutoxy)-2'-chlorobibenzyl hydrochloride, m.p. 122°-123° C.

後処理

  1. concentrationThe reaction mixture was concentrated and to the concentrate
  2. additionwas added 2 N-NaOH solution
  3. extractionThe product was extracted with ether
  4. washwashed well with saturated sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. additionTo the ether solution was added 20% ethanolic hydrogen chloride
  7. customto yield white crystals
  8. customRecrystallization from ethanol-ether

出典と根拠

ORDレコード
ord-aff028e2565840c482cd64f53b57f984
出典データセット
uspto-grants-1982_04
特許番号
US04323568

反応ノート

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