Potassium Iodide → 4-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester

HRID 511065ノート

反応式

HRID 511065 の反応式
[CH2:1]([O:3][C:4](=[O:9])[CH2:5][CH2:6][CH2:7]Br)[CH3:2].C(N(CC)CC)C.[F:17][C:18]([F:32])([F:31])[C:19]1[CH:24]=[CH:23][C:22]([N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[CH:21][CH:20]=1.[I-].[K+]>O1CCCC1.ClCCl>[CH2:1]([O:3][C:4](=[O:9])[CH2:5][CH2:6][CH2:7][N:28]1[CH2:27][CH2:26][N:25]([C:22]2[CH:21]=[CH:20][C:19]([C:18]([F:31])([F:32])[F:17])=[CH:24][CH:23]=2)[CH2:30][CH2:29]1)[CH3:2]

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 8471TriethylamineHCID 76300Ethyl 4-bromobutyrateHCID 1217181-(4-(Trifluoromethyl)phenyl)piperazine

生成物 1

HCID 585765934-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester収率 98%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Ethyl-4-bromobutyrate (390 mg, 2.00 mmol) and triethylamine (280 μL; 2.00 mmol) were added to a solution of 1-(4-trifluoromethylphenyl)-piperazine (460 mg; 2.00 mmol) in tetrahydrofuran (3 mL). Potassium iodide (332 mg; 2.00 mmol) was added and the resulting suspension is irradiated in a mono-mode microwave oven for 2 hours at 100° C. The suspension is then diluted with dichloromethane (15 mL) and washed twice with water (5 mL). The organic phase is then dried over sodium sulphate and is concentrated under reduced pressure to afford the desired product (660 mg; 1.96 mmol).

後処理

  1. customthe resulting suspension is irradiated in a mono-mode microwave oven for 2 hours at 100° C
  2. washwashed twice with water (5 mL)
  3. dry with materialThe organic phase is then dried over sodium sulphate
  4. concentrationis concentrated under reduced pressure

出典と根拠

ORDレコード
ord-3760a034e1e54b5895f97400fcb86c3d
出典データセット
uspto-grants-2015_08
特許番号
US09096524B2

反応ノート

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