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Dimethyl Sulfoxide → HCID 59730256, 화합물

HRID 492568
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HRID 492568 반응식
[F:1][C:2]1[C:16]([F:17])=[C:15]([CH:18]=[O:19])[CH:14]=[CH:13][C:3]=1[O:4][C:5]1[CH:12]=[CH:11][C:8]([C:9]#[N:10])=[CH:7][N:6]=1.C([O-])([O-])=[O:21].[K+].[K+].CS(C)=O>O>[F:1][C:2]1[C:16]([F:17])=[C:15]([CH:18]=[O:19])[CH:14]=[CH:13][C:3]=1[O:4][C:5]1[CH:12]=[CH:11][C:8]([C:9]([NH2:10])=[O:21])=[CH:7][N:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 679Dimethyl SulfoxideHCID 11430Potassium CarbonateHCID 59730380HCID 59730380, 화합물

생성물 1

HCID 59730256HCID 59730256, 화합물수율 148.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Add 30% aq. B202 (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. additionAdd 30% aq. B202 (7.95 ml)
  2. extractionextract with EtOAc
  3. washWash the
  4. extractionextract with water and brine
  5. dry with materialbefore drying (MgSO4)
  6. concentrationconcentrating

출처 및 근거

ORD 기록
ord-ac16a0aacd1e4e0dbd71520af2833c5c
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07531557B2

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