Dimethylamine → HCID 57713885、化合物

HRID 1984047ノート

反応式

HRID 1984047 の反応式
Cl[S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][C:13]=1[NH:14][CH3:15])[C:8]([OH:10])=[O:9])(=[O:4])=[O:3].C(OCC)(=O)C.[CH3:22][NH:23][CH3:24]>>[CH3:22][N:23]([CH3:24])[S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][C:13]=1[NH:14][CH3:15])[C:8]([OH:10])=[O:9])(=[O:4])=[O:3]

参加物

4

反応物 3

HCID 674DimethylamineHCID 8857Ethyl AcetateHCID 57713890HCID 57713890、化合物

生成物 1

HCID 57713885HCID 57713885、化合物収率 92%

実験手順

3-(Chlorosulfonyl)-4-(methylamino)benzoic acid (1.2, 0.515 g, 2.06 mmol) was dissolved in ethyl acetate (8 mL, 0.08 mol). Dimethylamine (0.4 mL, 0.008 mol) was added next. The reaction was left to stir for 4 hours. The reaction was extracted with 0.5 M HCl, washed with water and brine, and the organic layer dried over magnesium sulfate. The ethyl acetate was evaporated and the crude product 1.3.Af was obtained in 92% yield. MS analysis (m−1)=257.

後処理

  1. waitThe reaction was left
  2. extractionThe reaction was extracted with 0.5 M HCl
  3. washwashed with water and brine
  4. dry with materialthe organic layer dried over magnesium sulfate
  5. customThe ethyl acetate was evaporated
  6. customwas obtained in 92% yield

出典と根拠

ORDレコード
ord-594541c22e49437db4f254a9f996dd28
出典データセット
uspto-grants-2009_06
特許番号
US07544676B2

反応ノート

読み込み中…