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4-Methoxy-2,6-dimethylbenzene-1-sulfonyl chloride → HCID 59483781、化合物

HRID 1808372
ノート
印刷プレビュー

反応式

HRID 1808372 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH3:9])[C:6]([S:10](Cl)(=[O:12])=[O:11])=[C:5]([CH3:14])[CH:4]=1.Cl.[NH:16]1[C:24]2[C:19](=[CH:20][CH:21]=[C:22]([C:25]([O:27][CH3:28])=[O:26])[CH:23]=2)[CH2:18][CH2:17]1>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH3:9])[C:6]([S:10]([N:16]2[C:24]3[C:19](=[CH:20][CH:21]=[C:22]([C:25]([O:27][CH3:28])=[O:26])[CH:23]=3)[CH2:18][CH2:17]2)(=[O:12])=[O:11])=[C:5]([CH3:14])[CH:4]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 159174964-Methoxy-2,6-dimethylbenzene-1-sulfonyl chlorideHCID 53408435methyl 2,3-dihydro-1H-indole-6-carboxylate hydrochloride

生成物 1

HCID 59483781HCID 59483781、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
70 °C

実験手順

4-Methoxy-2,6-dimethylbenzene-1-sulfonyl chloride (1.3 g, 0.0056 mol) was added at 25° C., under argon, to a solution of methyl indoline-6-carboxylate hydrochloride (1.2 g, 0.0056 mol) in dry pyridine (12 ml), and the resulting reaction mixture was stirred overnight at 70° C. The solvent was removed in vacuo, and the residue was taken up in dichloromethane and washed with water (2×), saturated copper sulfate solution (2×) and saturated sodium chloride solution, then dried (Na2SO4) and concentrated in vacuo. The resulting crude product was purified by column chromatography (silica gel, 10-30% ethyl acetate in hexane). Yield: 1.9 g (90%)

後処理

  1. customthe resulting reaction mixture
  2. customThe solvent was removed in vacuo
  3. washwashed with water (2×), saturated copper sulfate solution (2×) and saturated sodium chloride solution
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo
  6. customThe resulting crude product was purified by column chromatography (silica gel, 10-30% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-c89a20c912424c5aaac407b55f990aca
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08357717B2

反応ノート

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