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Cesium carbonate → N-(4-methoxybenzyl)-2-(methoxymethyl)-3-oxo-N-(thiazol-2-yl)-3,4-dihydro-2H-benzo[b][1,4]oxazine-7-sulfonamide

HRID 528646
ノート
印刷プレビュー

反応式

HRID 528646 の反応式
Cl[CH:2]([CH2:6][O:7][CH3:8])[C:3](Cl)=[O:4].[NH2:9][C:10]1[CH:15]=[CH:14][C:13]([S:16]([N:19]([CH2:25][C:26]2[CH:31]=[CH:30][C:29]([O:32][CH3:33])=[CH:28][CH:27]=2)[C:20]2[S:21][CH:22]=[CH:23][N:24]=2)(=[O:18])=[O:17])=[CH:12][C:11]=1[OH:34].C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C.O>[CH3:33][O:32][C:29]1[CH:28]=[CH:27][C:26]([CH2:25][N:19]([C:20]2[S:21][CH:22]=[CH:23][N:24]=2)[S:16]([C:13]2[CH:14]=[CH:15][C:10]3[NH:9][C:3](=[O:4])[CH:2]([CH2:6][O:7][CH3:8])[O:34][C:11]=3[CH:12]=2)(=[O:18])=[O:17])=[CH:31][CH:30]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10796Cesium carbonateHCID 874933872-Chloro-3-methoxypropanoyl chlorideHCID 89761412HCID 89761412、化合物

生成物 1

HCID 89761918N-(4-methoxybenzyl)-2-(methoxymethyl)-3-oxo-N-(thiazol-2-yl)-3,4-dihydro-2H-benzo[b][1,4]oxazine-7-sulfonamide収率 39.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

実験手順

To a solution of 2-chloro-3-methoxypropanoyl chloride (500 mg, 3.18 mmol) and 4-amino-3-hydroxy-N-(4-methoxybenzyl)-N-(thiazol-2-yl)benzenesulfonamide (Intermediate AD; 1.04 g, 2.65 mmol) in DMF (20 mL) was added Cs2CO3 (2.59 g, 7.95 mmol). The reaction mixture was stirred at ambient temperature for 16 h. The reaction mixture was diluted with water (200 mL) and extracted with ethyl acetate (2×100 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated under reduced pressure to obtain the crude material which was further purified by column chromatography (silica gel 100-200 mesh and 0-30% ethyl acetate in hexane) to obtain N-(4-methoxybenzyl)-2-(methoxymethyl)-3-oxo-N-(thiazol-2-yl)-3,4-dihydro-2H-benzo[b][1,4]oxazine-7-sulfonamide (500 mg, 33.1%) as an off white solid. m/z (ESI) 476.1 (M+H)+.

後処理

  1. extractionextracted with ethyl acetate (2×100 mL)
  2. dry with materialThe combined organic layers were dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customto obtain the crude material which
  6. customwas further purified by column chromatography (silica gel 100-200 mesh and 0-30% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-f1aa88aba60b48749d4e3ab44692943f
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09346798B2

反応ノート

読み込み中…

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