Acetyl chloride → HCID 68954629、化合物

HRID 750992ノート

反応式

HRID 750992 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([N:10]([CH2:20][C:21]2[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=2)[C:11]2[CH:12]=[C:13]([CH:17]=[CH:18][CH:19]=2)[C:14]([OH:16])=[O:15])[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].[C:27](Cl)(=O)C>CO>[OH:1][C:2]1[CH:3]=[C:4]([N:10]([CH2:20][C:21]2[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=2)[C:11]2[CH:12]=[C:13]([CH:17]=[CH:18][CH:19]=2)[C:14]([O:16][CH3:27])=[O:15])[CH:5]=[CH:6][C:7]=1[O:8][CH3:9]

参加物

4

反応物 2

HCID 6367Acetyl chlorideHCID 10360501Benzoic acid, 3-[(3-hydroxy-4-methoxyphenyl)(3-pyridinylmethyl)amino]-

生成物 1

HCID 68954629HCID 68954629、化合物収率 84%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

N-(3-Hydroxy-4-methoxyphenyl)-N-(3-pyridylmethyl)-3-aminobenzoic acid (7.0 g, 20.0 mmol) was dissolved in 210 mL of MeOH and 2.8 g (36.0 mmol) of acetyl chloride was added. The material was warmed to reflux with stirring overnight. The solution was concentrated in vacuo and then diluted with 200 mL of DCM and washed with saturated NaHCO3, brine, dried (Na2SO4), and concentrated to give 6.85 g (84% yield) of the desired target.

後処理

  1. temperatureThe material was warmed
  2. temperatureto reflux
  3. concentrationThe solution was concentrated in vacuo
  4. additiondiluted with 200 mL of DCM
  5. washwashed with saturated NaHCO3, brine
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated
  8. customto give 6.85 g (84% yield) of the desired target

出典と根拠

ORDレコード
ord-7d7a9209c99543d7addca56ae8930622
出典データセット
uspto-grants-2008_07
特許番号
US07405230B2

反応ノート

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