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

HRID 1257759노트

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HRID 1257759 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-3cc46c5071d847278e2a9172d0e880b2
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08461328B2

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