Acetyl chloride → 4-(4-Methylpiperazin-1-yl)phenyl acetate

HRID 45807

反応式

HRID 45807 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1.[C:15](Cl)(=[O:17])[CH3:16]>C(Cl)Cl>[C:15]([O:14][C:11]1[CH:12]=[CH:13][C:8]([N:5]2[CH2:4][CH2:3][N:2]([CH3:1])[CH2:7][CH2:6]2)=[CH:9][CH:10]=1)(=[O:17])[CH3:16]

参加物

4

反応物 2

HCID 6367Acetyl chlorideHCID 116224864-(4-Methyl-1-piperazinyl)phenol

生成物 1

HCID 679737964-(4-Methylpiperazin-1-yl)phenyl acetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 4-(4-methylpiperazin-1-yl)phenol 1.080 mg (5.59 mmol) and TEA 1.72 ml (12.3 mmol) in DCM was cooled in an ice bath and 0.44 ml (6.15 mmol) of acetyl chloride were added dropwise. After completion, the reaction was filtered, the organic phase quickly extracted with water, dried over Na2SO4 and evaporated down to give a light pink solid. LC/MS (m/z): 235.4 [M+H]+, HPLC (254 nm) method 3 Rt 1.89 min.

後処理

  1. temperaturewas cooled in an ice bath
  2. filtrationAfter completion, the reaction was filtered
  3. extractionthe organic phase quickly extracted with water
  4. dry with materialdried over Na2SO4
  5. customevaporated down
  6. customto give a light pink solid

出典と根拠

ORDレコード
ord-ceedaa7f8b0344ddb93c9ecc488533c5
出典データセット
uspto-grants-2013_09
特許番号
US08541576B2

関連ノート

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