Methanol → Methyl 4-sulphamoylbenzoate

HRID 331187ノート

反応式

HRID 331187 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-ca03cd80393e45acabaefc161bf7241a
出典データセット
uspto-grants-2014_11
特許番号
US08877757B2

反応ノート

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