Water → 4-(6-Benzenesulfonyl-6H-1,2,3,5,6-pentaaza-as-indacen-1-yl)-1-methyl-cyclohexanol

HRID 1257759ノート

反応式

HRID 1257759 の反応式
[C:1]1([S:7]([N:10]2[CH:21]=[CH:20][C:19]3[C:11]2=[N:12][CH:13]=[C:14]2[C:18]=3[N:17]([CH:22]3[CH2:27][CH2:26][C:25](=[O:28])[CH2:24][CH2:23]3)[N:16]=[N:15]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Br].[CH3:30][Mg].O>O1CCCC1>[C:1]1([S:7]([N:10]2[CH:21]=[CH:20][C:19]3[C:11]2=[N:12][CH:13]=[C:14]2[C:18]=3[N:17]([CH:22]3[CH2:23][CH2:24][C:25]([CH3:30])([OH:28])[CH2:26][CH2:27]3)[N:16]=[N:15]2)(=[O:8])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 962WaterHCID 673431594-(6-Benzenesulfonyl-6H-1,2,3,5,6-pentaaza-as-indacen-1-yl)-cyclohexanoneHCID 178419573HCID 178419573、化合物

生成物 1

HCID 673445664-(6-Benzenesulfonyl-6H-1,2,3,5,6-pentaaza-as-indacen-1-yl)-1-methyl-cyclohexanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a solution of 4-(6-Benzenesulfonyl-6H-1,2,3,5,6-pentaaza-as-indacen-1-yl)-cyclohexanone (400 mg, 1.01 mmol) in anhydrous tetrahydrofuran (20 mL) was added dropwise methylmagnesium bromine (3 M in diethyl ether, 2.3 mL, 7.07 mmol), followed by stirring at 0° C. for 30 minutes under nitrogen. The reaction was warmed to room temperature and stirred for another 90 minutes. The resulting mixture was poured into water and extracted with ethyl acetate. The organic solution was used for the next step. LCMS (Method K, ESI): RT=1.318 min and 1.359, m+H=411.8.

後処理

  1. temperatureThe reaction was warmed to room temperature
  2. stirringstirred for another 90 minutes
  3. extractionextracted with ethyl acetate

出典と根拠

ORDレコード
ord-3cc46c5071d847278e2a9172d0e880b2
出典データセット
uspto-grants-2013_06
特許番号
US08461328B2

反応ノート

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