Methanesulfonyl chloride → 4-Benzoyl-1-methanesulphonylpiperidine

HRID 900757

反応式

HRID 900757 の反応式
CCN(C(C)C)C(C)C.Cl.[C:11]1([C:17]([CH:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)=[O:18])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[CH3:25][S:26](Cl)(=[O:28])=[O:27]>C(Cl)Cl>[CH3:25][S:26]([N:22]1[CH2:23][CH2:24][CH:19]([C:17]([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)=[O:18])[CH2:20][CH2:21]1)(=[O:28])=[O:27]

参加物

5

反応物 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 27244374-Benzoylpiperidine hydrochloride

生成物 1

HCID 160435364-Benzoyl-1-methanesulphonylpiperidine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Neat DIPEA (1.54 ml, 8.86 mmol) was added dropwise to a solution of phenyl(4-piperidinyl)methanone hydrochloride (1 g, 4.43 mmol) in CH2Cl2 (20 ml) at 0° C. Then, neat MsCl (377 μL, 4.87 mmol) was slowly added and the cooling bath was removed. After 30 minutes, the reaction was quenched with water and diluted with CH2Cl2. After separation, the organic phase was washed with brine, dried over MgSO4 and evaporated to dryness. The final ketone 1 was obtained as a white solid (1.16 g, 98%).

後処理

  1. customthe cooling bath was removed
  2. customthe reaction was quenched with water
  3. additiondiluted with CH2Cl2
  4. customAfter separation
  5. washthe organic phase was washed with brine
  6. dry with materialdried over MgSO4
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-aa78a692c2cb4f939b8c603d3c78b629
出典データセット
uspto-grants-2008_04
特許番号
US07361668B2

関連ノート

読み込み中…