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Sodium Acetate → HCID 10117620, 화합물

HRID 1791123
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HRID 1791123 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH:9]=[C:10]([C:15](=O)[CH2:16][CH2:17][N:18]1[CH2:22][CH2:21][S:20][CH2:19]1)[C:11]([O:13][CH3:14])=[O:12].Cl.[F:25][C:26]1[C:27]([C:33](=[NH:35])[NH2:34])=[N:28][CH:29]=[C:30]([F:32])[CH:31]=1.C([O-])(=O)C.[Na+]>C(O)(C)C>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH:9]1[C:10]([C:11]([O:13][CH3:14])=[O:12])=[C:15]([CH2:16][CH2:17][N:18]2[CH2:22][CH2:21][S:20][CH2:19]2)[NH:35][C:33]([C:27]2[C:26]([F:25])=[CH:31][C:30]([F:32])=[CH:29][N:28]=2)=[N:34]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 517045Sodium AcetateHCID 220278403,5-Difluoropyridine-2-carboximidamide--hydrogen chloride (1/1)HCID 69588140HCID 69588140, 화합물

생성물 1

HCID 10117620HCID 10117620, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A solution of 0.20 g (0.56 mmol) of the compound from Example IX in 5 ml of isopropanol is heated together with 0.11 g (0.56 mmol) of the compound from Example VI and 0.06 g (0.67 mmol) of sodium acetate under reflux for 2 hours. The reaction mixture is concentrated, and the residue is taken up in ethyl acetate and extracted with dilute hydrochloric acid. The aqueous phase is made alkaline with dilute sodium hydroxide solution and extracted with ethyl acetate. The organic phase is dried over sodium sulfate and concentrated. The residue is chromatographed on silica gel with cyclohexane/ethyl acetate (5:1→3:1) as mobile phase.

후처리

  1. temperatureunder reflux for 2 hours
  2. concentrationThe reaction mixture is concentrated
  3. extractionextracted with dilute hydrochloric acid
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic phase is dried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue is chromatographed on silica gel with cyclohexane/ethyl acetate (5:1→3:1) as mobile phase

출처 및 근거

ORD 기록
ord-2fba051fc5664ebf804df2ddb251efca
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07074784B2

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