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

HRID 446858노트

반응식

HRID 446858 반응식
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]

참가 물질

5

반응물 3

HCID 887MethanolHCID 962WaterHCID 68494934HCID 68494934, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-78b286e9214246a0adcbb984ffcb41ea
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481527B2

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