Methanol → Methyl 4-sulphamoylbenzoate

HRID 655614ノート

反応式

HRID 655614 の反応式
[NH2:1][S:2]([C:5]1[CH:13]=[CH:12][C:8]([C:9]([OH:11])=[O:10])=[CH:7][CH:6]=1)(=[O:4])=[O:3].S(Cl)(Cl)=O.[CH3:18]O>>[NH2:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([C:9]([O:11][CH3:18])=[O:10])=[CH:12][CH:13]=1)(=[O:3])=[O:4]

参加物

4

反応物 3

HCID 887MethanolHCID 8739CarzenideHCID 24386Thionyl Chloride

生成物 1

HCID 89847Methyl 4-sulphamoylbenzoate収率 75%

実験手順

To a suspension of 4-(aminosulfonyl)benzoic acid (500 mg, 2.5 mmol) in MeOH (2 ml) at 0° C. is added thionylchloride (0.2 ml, 7.4 mmol). The reaction mixture is stirred at rt overnight. When TLC confirms the total consumption of the starting acid, the solvent and excess thionyl chloride are removed under reduced pressure to afford 400 mg (75%) of the title compound, which was used in the next step without any further purification. LC/MS: (ES+):215.9, (ES−):214.1.

後処理

  1. customthe total consumption of the starting acid
  2. customthe solvent and excess thionyl chloride are removed under reduced pressure

出典と根拠

ORDレコード
ord-e6c34b6f574d4834a2b979ebaca7a874
出典データセット
uspto-grants-2011_12
特許番号
US08071597B2

反応ノート

読み込み中…