Methylamine → 4-chloro-2-(hydroxymethyl)-N-methylbenzamide

HRID 2252817ノート

反応式

HRID 2252817 の反応式
[CH3:1][NH2:2].[Cl:3][C:4]1[CH:13]=[CH:12][C:7]2[C:8](=[O:11])[O:9][CH2:10][C:6]=2[CH:5]=1>CO>[Cl:3][C:4]1[CH:13]=[CH:12][C:7]([C:8]([NH:2][CH3:1])=[O:11])=[C:6]([CH2:10][OH:9])[CH:5]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 2417375-Chloro-1,3-dihydro-2-benzofuran-1-one

生成物 1

HCID 691802354-chloro-2-(hydroxymethyl)-N-methylbenzamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Methylamine gas was condensed into a sealed tube at −78° C., and a solution of 5-chloro-2-benzofuran-1(3H)-one (6.68 g, 39.8 mmol) in methanol (30 mL) was added. The solution was slowly warmed to room temperature overnight; The reaction was concentrated in vacuo, and the residue was partitioned between water and and chloroform. After three extractions with chloroform, the combined organics were dried over sodium sulfate, filtered, and concentrated in vacuo to afford 4-chloro-2-(hydroxymethyl)-N-methylbenzamide.

後処理

  1. customcondensed into a sealed tube at −78° C.
  2. concentrationThe reaction was concentrated in vacuo
  3. customthe residue was partitioned between water and and chloroform
  4. extractionAfter three extractions with chloroform
  5. dry with materialthe combined organics were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-55e528e2c8444b6191108304948f3a54
出典データセット
uspto-grants-2008_01
特許番号
US07323460B2

反応ノート

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