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Ethanol → 5-Isothiazol-5-yl-4'-methyl-biphenyl-3-carboxylic acid (2-methoxy-1-methyl-ethyl)-amide

HRID 1888921
ノート
印刷プレビュー

反応式

HRID 1888921 の反応式
[CH3:1][O:2][CH2:3][CH:4]([NH:6][C:7]([C:9]1[CH:10]=[C:11]([C:22]2[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][CH:23]=2)[CH:12]=[C:13]([C:15](=[S:21])[CH:16]=[CH:17][N:18](C)C)[CH:14]=1)=[O:8])[CH3:5].C(O)C.CO.OOS(N)(=O)=O>N1C=CC=CC=1>[CH3:1][O:2][CH2:3][CH:4]([NH:6][C:7]([C:9]1[CH:10]=[C:11]([C:22]2[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][CH:23]=2)[CH:12]=[C:13]([C:15]2[S:21][N:18]=[CH:17][CH:16]=2)[CH:14]=1)=[O:8])[CH3:5]
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 4

HCID 702EthanolHCID 887MethanolHCID 16204977hydroxyl-amine-O-sulfonic acidHCID 722974795-(3-Dimethylamino-thioacryloyl)-4'-methyl-biphenyl-3-carboxylic acid (2-methoxy-1-methyl-ethyl)-amide

生成物 1

HCID 251695065-Isothiazol-5-yl-4'-methyl-biphenyl-3-carboxylic acid (2-methoxy-1-methyl-ethyl)-amide収率 50%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a 0° C. solution of 5-(3-dimethylamino-thioacryloyl)-4′-methyl-biphenyl-3-carboxylic acid (2-methoxy-1-methyl-ethyl)-amide (200 mg, 0.505 mmol) in a mixture of pyridine (80 uL), ethanol (3 mL) and MeOH (1 mL) was added hydroxyl-amine-O-sulfonic acid (0.76 mmol, 85.7 mg) in one portion. The reaction mixture was stirred for two hours, during which time the mixture was allowed to warm to room temperature. Solvent was removed in vacuo, and the residue was subjected to Preparative HPLC for separation to give 92 mg (50%) of 5-isothiazol-5-yl-4′-methyl-biphenyl-3-carboxylic acid (2-methoxy-1-methyl-ethyl)-amide, MS (M+H)=367.

後処理

  1. customSolvent was removed in vacuo
  2. customthe residue was subjected to Preparative HPLC for separation

出典と根拠

ORDレコード
ord-a7a8013db34346b5bde672ae00abe496
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08501933B2

反応ノート

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