Piperazine → 1-(2,4-Difluorobenzyl)piperazine

HRID 713199ノート

反応式

HRID 713199 の反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[CH2:8][C:9]1[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=1[F:16]>C1COCC1>[F:16][C:10]1[CH:11]=[C:12]([F:15])[CH:13]=[CH:14][C:9]=1[CH2:8][N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 4837PiperazineHCID 27369481-(Chloromethyl)-2,4-difluorobenzene

生成物 1

HCID 27828061-(2,4-Difluorobenzyl)piperazine収率 92%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

A mixture of piperazine (26.5 g, 308 mmol) in THF (350 mL) was heated to 70° C. and 1-(chloromethyl)-2,4-difluorobenzene (5 g, 30.8 mmol) was added. The suspension was heated at 70° C. overnight. The solid (piperazine) was filtered off, and the solvent was removed under reduced pressure. The residue was partitioned between EtOAc and water. The organic layer was dried and concentrated to give the title compound (6 g, 92%). ESI-MS m/z [M+H]+ 213.04.

後処理

  1. temperatureThe suspension was heated at 70° C. overnight
  2. filtrationThe solid (piperazine) was filtered off
  3. customthe solvent was removed under reduced pressure
  4. customThe residue was partitioned between EtOAc and water
  5. customThe organic layer was dried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-4c0d105bcc774bf7843a0cf0aaa34a63
出典データセット
uspto-grants-2015_11
特許番号
US09181249B2

反応ノート

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