Methanesulfonyl chloride → 5-Mesylamino-3-(quinol-4-ylmethylene)-2-oxindole

HRID 356992ノート

反応式

HRID 356992 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6](=[O:11])[C:5]2=[CH:12][C:13]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[N:16]=[CH:15][CH:14]=1.[S:23](Cl)([CH3:26])(=[O:25])=[O:24]>N1C=CC=CC=1>[S:23]([NH:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6](=[O:11])[C:5]2=[CH:12][C:13]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[N:16]=[CH:15][CH:14]=1)([CH3:26])(=[O:25])=[O:24]

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 545367025-Amino-3-(quinol-4-ylmethylene)-2-oxindole

生成物 1

HCID 676153715-Mesylamino-3-(quinol-4-ylmethylene)-2-oxindole収率 70%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a stirred solution of 5-amino-3-(quinol-4-ylmethylene)-2-oxindole (2.873 g, 10 mmol) in pyridine (10 ml) was added gradually mesylchloride (1.146 g, 10 mmol) at 0°-5° C. under cooling. The reaction mixture was stirred for about 5 h at 0°-5° C. and then for 15 hours at room temperature. The mixture was poured onto an ice-water mixture, the precipitate filtered off, the residue washed thoroughly with water and then chromatographed on silica gel using CHCl3 --MeOH mixtures as eluant. Thus pure title compound was obtained in about 70% yield.

後処理

  1. temperatureunder cooling
  2. waitfor 15 hours at room temperature
  3. filtrationthe precipitate filtered off
  4. washthe residue washed thoroughly with water
  5. customchromatographed on silica gel

出典と根拠

ORDレコード
ord-ec00d732ae1f4797a0ea72a0b1697788
出典データセット
uspto-grants-1998_11
特許番号
US05840745

反応ノート

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