Hydrochloric Acid → 1-[3-(Chloromethyl)benzoyl]piperidine

HRID 1721601ノート

反応式

HRID 1721601 の反応式
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:7][CH2:8][C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12](Cl)=[O:13].Cl>O1CCCC1>[Cl:7][CH2:8][C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12]([N:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)=[O:13]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 8082PiperidineHCID 27333243-(Chloromethyl)benzoyl chloride

生成物 1

HCID 100144051-[3-(Chloromethyl)benzoyl]piperidine収率 86,436.797%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To an ice-cooled solution of piperidine (67.6 g, 0.793 mole) in tetrahydrofuran (1 L) was added dropwise a solution of 3-chloromethylbenzoyl chloride (100.0 g, 0.529 mmol). When the addition was complete, the reaction mixture was allowed to warm to ambient temperature and was left to stir overnight. The reaction mixture was poured into a solution of 1N hydrochloric acid. This solution was extracted with diethyl ether. The ether extracts were combined, washed with water, dried (MgSO4), and concentrated to afford 108.7 g (86%) of N-(3-(chloromethyl)benzoyl)piperidine (10) as a pale yellow oil whose 1H NMR in CDCl3 supported the structure.

後処理

  1. additionWhen the addition
  2. waitwas left
  3. extractionThis solution was extracted with diethyl ether
  4. washwashed with water
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-109c7b41765d40ada47037098d6823a0
出典データセット
uspto-grants-1996_04
特許番号
US05512566

反応ノート

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