Water → 3-methyl-4-[2-[N-(5-methyl-2-furylsulfonyl)amino]4,5-dimethylphenoxymethyl]benzoic acid methyl ester

HRID 415705ノート

反応式

HRID 415705 の反応式
[CH3:1][O:2][C:3](=[O:22])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][O:11][C:12]2[CH:17]=[C:16]([CH3:18])[C:15]([CH3:19])=[CH:14][C:13]=2[NH2:20])=[C:6]([CH3:21])[CH:5]=1.[CH3:23][C:24]1[O:28][C:27]([S:29](Cl)(=[O:31])=[O:30])=[CH:26][CH:25]=1.C(OCC)(=O)C.O>N1C=CC=CC=1>[CH3:1][O:2][C:3](=[O:22])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][O:11][C:12]2[CH:17]=[C:16]([CH3:18])[C:15]([CH3:19])=[CH:14][C:13]=2[NH:20][S:29]([C:27]2[O:28][C:24]([CH3:23])=[CH:25][CH:26]=2)(=[O:31])=[O:30])=[C:6]([CH3:21])[CH:5]=1

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 178643615-Methylfuran-2-sulfonyl chlorideHCID 588919054-(2-amino-4,5-dimethylphenoxymethyl)-3-methylbenzoic Acid Methyl Ester

生成物 1

HCID 588919093-methyl-4-[2-[N-(5-methyl-2-furylsulfonyl)amino]4,5-dimethylphenoxymethyl]benzoic acid methyl ester

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
0 °C

実験手順

A solution of 4-(2-amino-4,5-dimethylphenoxymethyl)-3-methylbenzoic acid methyl ester prepared in Reference Example 2 (632 mg) in pyridine (4 ml) was cooled to 0° C., then 5-methylfuran-2-sulfonyl chloride (490 mg) was added dropwise thereto. After the solution was stirred for 1 hour at room temperature, the reaction mixture was diluted by ethyl acetate, and poured into water. The organic layer was washed, dried, concentrated under reduced pressure. The residue was washed by mixed solvent of diisopropylether and hexane to give the title compound (875 mg) having the following physical data.

後処理

  1. washThe organic layer was washed
  2. customdried
  3. concentrationconcentrated under reduced pressure
  4. washThe residue was washed
  5. additionby mixed solvent of diisopropylether and hexane

出典と根拠

ORDレコード
ord-6cac3a2d10d84936b55a8e130e55b8d7
出典データセット
uspto-grants-2012_01
特許番号
US08088802B2

反応ノート

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