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Dimethyl Sulfoxide → HCID 59730256, 화합물

HRID 228414
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반응식

HRID 228414 반응식
OO.[F:3][C:4]1[C:18]([F:19])=[C:17]([CH:20]=[O:21])[CH:16]=[CH:15][C:5]=1[O:6][C:7]1[CH:14]=[CH:13][C:10]([C:11]#[N:12])=[CH:9][N:8]=1.C([O-])([O-])=[O:23].[K+].[K+].CS(C)=O>O>[F:3][C:4]1[C:18]([F:19])=[C:17]([CH:20]=[O:21])[CH:16]=[CH:15][C:5]=1[O:6][C:7]1[CH:14]=[CH:13][C:10]([C:11]([NH2:12])=[O:23])=[CH:9][N:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 784Hydrogen PeroxideHCID 11430Potassium CarbonateHCID 59730380HCID 59730380, 화합물

생성물 1

HCID 59730256HCID 59730256, 화합물수율 148.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Add 30% aq. H2O2 (7.95 ml) to a suspension of 6-(2,3-difluoro-4-formyl-phenoxy)-nicotinonitrile (2.07 g, 7.95 mmol), K2CO3 (550 mg, 3.98 mmol) and DMSO (20 ml) stirring in an ice/water bath. After one hour, pour the reaction mixture into water and extract with EtOAc. Wash the extract with water and brine before drying (MgSO4) and concentrating to give 6-(2,3-difluoro-4-formyl-phenoxy)-nicotinamide (1.64 g) as a white solid. 1HNMR (DMSO-d6): 10.14 (s, 1H), 8.58 (s, 1H), 8.33 (d, 1H), 8.07 (s, 1H), 7.74 (t, 1H), 7.55 (s, 1H), 7.33 (d, 1H), 7.27 (t, 1H).

후처리

  1. extractionextract with EtOAc
  2. washWash the
  3. extractionextract with water and brine
  4. dry with materialbefore drying (MgSO4)
  5. concentrationconcentrating

출처 및 근거

ORD 기록
ord-fe63e056bf64492b8343e828ca55089a
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07560463B2

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