[[(Aminooxy)carbonyl](methyl)amino]methane hydrochloride → [(Z)-[3-[[2-(4-fluorophenyl)-2-hydroxyethyl]-methylsulfamoyl]-5,6-dihydro-4H-1-benzothiophen-7-ylidene]amino] N,N-dimethylcarbamate

HRID 1351330노트

반응식

HRID 1351330 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:25])[CH2:9][N:10]([CH3:24])[S:11]([C:14]2[C:15]3[CH2:22][CH2:21][CH2:20][C:19](=O)[C:16]=3[S:17][CH:18]=2)(=[O:13])=[O:12])=[CH:4][CH:3]=1.Cl.[NH2:27][O:28][C:29]([N:31]([CH3:33])[CH3:32])=[O:30]>C(O)(=O)C>[CH3:32][N:31]([CH3:33])[C:29]([O:28]/[N:27]=[C:19]1/[CH2:20][CH2:21][CH2:22][C:15]2[C:14]([S:11]([N:10]([CH2:9][CH:8]([C:5]3[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=3)[OH:25])[CH3:24])(=[O:12])=[O:13])=[CH:18][S:17][C:16]/1=2)=[O:30]

참가 물질

4

반응물 2

HCID 21098721[[(Aminooxy)carbonyl](methyl)amino]methane hydrochlorideHCID 77617953HCID 77617953, 화합물

생성물 1

HCID 11431333[(Z)-[3-[[2-(4-fluorophenyl)-2-hydroxyethyl]-methylsulfamoyl]-5,6-dihydro-4H-1-benzothiophen-7-ylidene]amino] N,N-dimethylcarbamate

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

7-Oxo-4,5,6,7-tetrahydro-benzo[b]thiophene-3-sulfonic acid [2-(4-fluorophenyl)-2-hydroxyethyl]-methyl-amide (the compound of Preparation Example 48) (60 mg) and [[(aminooxy)carbonyl](methyl)amino]methane hydrochloride (the compound of Preparation Example 122) (24 mg) were stirred in acetic acid at 50° C. for 3 hours. The residue resulting from the removal of the solvent by evaporation was purified by silica gel column chromatography (hexane/ethyl acetate). Among the two spots that were identifeid by developing the reaction solution by TLC (solvent system was hexane:ethyl acetate=1:3), the fraction of the compound with a high polarity (low Rf value) was collected, and the title compound (9 mg) was obtained as a colorless amorphous substance.

후처리

  1. customthe compound of Preparation Example 122) (24 mg)
  2. customThe residue resulting from the removal of the solvent by evaporation
  3. customwas purified by silica gel column chromatography (hexane/ethyl acetate)
  4. customthe fraction of the compound with a high polarity (low Rf value) was collected

출처 및 근거

ORD 기록
ord-79074fe338cd44a7bda11ac704c23b0e
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217723B2

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