Methanol → {4-[2-(2,4-Dichloro-phenoxy)-phenylsulfamoyl]-benzoylamino}-acetic acid

HRID 446858ノート

反応式

HRID 446858 の反応式
C([O:3][C:4](=[O:34])[CH2:5][NH:6][C:7](=[O:33])[C:8]1[CH:13]=[CH:12][C:11]([S:14](=[O:32])(=[O:31])[NH:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[O:22][C:23]2[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][C:24]=2[Cl:30])=[CH:10][CH:9]=1)C.O.CO>O1CCCC1>[Cl:30][C:24]1[CH:25]=[C:26]([Cl:29])[CH:27]=[CH:28][C:23]=1[O:22][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[NH:15][S:14]([C:11]1[CH:12]=[CH:13][C:8]([C:7]([NH:6][CH2:5][C:4]([OH:34])=[O:3])=[O:33])=[CH:9][CH:10]=1)(=[O:31])=[O:32]

参加物

5

反応物 3

HCID 887MethanolHCID 962WaterHCID 68494934HCID 68494934、化合物

生成物 1

HCID 68493493{4-[2-(2,4-Dichloro-phenoxy)-phenylsulfamoyl]-benzoylamino}-acetic acid収率 93%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of {4-[2-(2,4-dichloro-phenoxy)-phenylsulfamoyl]-benzoylamino}-acetic acid ethyl ester (7.68 g, 14.67 mmol) in a mixture of tetrahydrofuran (36 mL), water (18 mL) and methanol (18 mL) lithium hydroxide monohydrate (3.09 g, 73.64 mmol) was added and the reaction mixture was stirred at room temperature for 2 h. The mixture was concentrated, the residue was dissolved in water, acidified with 1M hydrochloric acid, the precipitated solid was filtered off, washed with water and dried to yield 6.76 g (93%) of the title compound as a yellowish solid. MS (EI) 496.2 (MH+).

後処理

  1. additionwas added
  2. concentrationThe mixture was concentrated
  3. dissolutionthe residue was dissolved in water
  4. filtrationthe precipitated solid was filtered off
  5. washwashed with water
  6. customdried

出典と根拠

ORDレコード
ord-78b286e9214246a0adcbb984ffcb41ea
出典データセット
uspto-grants-2013_07
特許番号
US08481527B2

反応ノート

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