Dichloromethane → 1-(3-Chlorophenyl)piperazine

HRID 1405435ノート

反応式

HRID 1405435 の反応式
CO[C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.C(=O)(O)[O-].[Na+].[Cl:27]CCl>FC(F)(F)C(O)=O>[Cl:27][C:4]1[CH:5]=[C:6]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:7]=[CH:8][CH:3]=1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 516892Sodium BicarbonateHCID 10935225tert-butyl 4-(4-methoxyphenyl)piperazine-1-carboxylate

生成物 1

HCID 13551-(3-Chlorophenyl)piperazine収率 50%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
20 °C

実験手順

A solution of t-butyl 4-(4-methoxyphenyl)piperazine-1-carboxylate (1.3 g, 4.39 mmol, 1.00 equiv) in dichloromethane (11 mL) and trifluoroacetic acid (6 mL) was placed in a 50-mL round bottom flask and stirred for 3 h at 20° C. in an oil bath. The solution was adjusted to a pH value of 7-8 with a saturated aqueous solution of sodium bicarbonate, and extracted with 6×15 mL of dichloromethane. The organic layers combined and dried over anhydrous sodium sulfate, filtered to remove solids, and concentrated under vacuum yielding 430 mg (50%) of 1-(3-chlorophenyl)piperazine as a yellow solid.

後処理

  1. extractionextracted with 6×15 mL of dichloromethane
  2. dry with materialdried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. customto remove solids
  5. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-d0ac1a3959284372888db603c260d124
出典データセット
uspto-grants-2014_12
特許番号
US08916560B2

反応ノート

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