O,O-Dipyridin-2-yl carbonothioate → HCID 87182869, 화합물

HRID 252655

반응식

HRID 252655 반응식
[CH3:1][S:2][C:3]1[N:8]=[C:7]([C:9]2[C:10]([O:15][C:16]3[CH:17]=[CH:18][C:19]([NH2:22])=[N:20][CH:21]=3)=[N:11][CH:12]=[CH:13][CH:14]=2)[CH:6]=[CH:5][N:4]=1.C1C=C(O[C:30](OC2N=CC=CC=2)=[S:31])N=CC=1>C(Cl)Cl>[N:22]([C:19]1[N:20]=[CH:21][C:16]([O:15][C:10]2[C:9]([C:7]3[CH:6]=[CH:5][N:4]=[C:3]([S:2][CH3:1])[N:8]=3)=[CH:14][CH:13]=[CH:12][N:11]=2)=[CH:17][CH:18]=1)=[C:30]=[S:31]

참가 물질

4

반응물 2

HCID 719784O,O-Dipyridin-2-yl carbonothioateHCID 668627075-(3-(2-(Methylthio)pyrimidin-4-yl)pyridin-2-yloxy)pyridin-2-amine

생성물 1

HCID 87182869HCID 87182869, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a mixture of 5-(3-(2-(methylthio)pyrimidin-4-yl)pyridin-2-yloxy)pyridin-2-amine (0.170 g, 0.546 mmol) in DCM was added di-2-pyridyl thionocarbonate (0.133 g, 0.573 mmol). The reaction was allowed to stir overnight. After 16 h, the reaction was washed 4× with water, then transferred to a separatory funnel and diluted with DCM. The organic layer was washed with water, dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to give 4-(2-(6-isothiocyanatopyridin-3-yloxy)pyridin-3-yl)-2-(methylthio)pyrimidine. MS m/z=354 [M+H]+. Calc'd for C16H11N5OS2: 353.4.

후처리

  1. waitAfter 16 h
  2. washthe reaction was washed 4× with water
  3. customtransferred to a separatory funnel
  4. additiondiluted with DCM
  5. washThe organic layer was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-9afbacac2bde423297e73518ecc57ec3
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07868177B2

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