홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Sodium hydride → 6-chloro-[[2-methyl-3-oxo-7-(4-propan-2-ylpiperazin-1-yl)-1H-isoindol-4-yl]amino]pyridine-3-carbonitrile

HRID 1045909
노트
인쇄 미리보기

반응식

HRID 1045909 반응식
[H-].[Na+].[NH2:3][C:4]1[CH:5]=[CH:6][C:7]([N:15]2[CH2:20][CH2:19][N:18]([CH:21]([CH3:23])[CH3:22])[CH2:17][CH2:16]2)=[C:8]2[C:12]=1[C:11](=[O:13])[N:10]([CH3:14])[CH2:9]2.Cl[C:25]1[CH:30]=[C:29]([Cl:31])[N:28]=[CH:27][C:26]=1[C:32]#[N:33]>C1COCC1.CCOC(C)=O>[Cl:31][C:29]1[N:28]=[C:27]([NH:3][C:4]2[CH:5]=[CH:6][C:7]([N:15]3[CH2:16][CH2:17][N:18]([CH:21]([CH3:23])[CH3:22])[CH2:19][CH2:20]3)=[C:8]3[C:12]=2[C:11](=[O:13])[N:10]([CH3:14])[CH2:9]3)[C:26]([C:32]#[N:33])=[CH:25][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 455880804,6-Dichloropyridine-3-carbonitrileHCID 598492047-amino-2-methyl-4-(4-propan-2-ylpiperazin-1-yl)-3H-isoindol-1-one

생성물 1

HCID 866551346-chloro-[[2-methyl-3-oxo-7-(4-propan-2-ylpiperazin-1-yl)-1H-isoindol-4-yl]amino]pyridine-3-carbonitrile수율 21.4%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran
용매
HCID 8857Ethyl Acetate용매

실험 절차

Sodium hydride (0.557 g, 13.93 mmol) was added portionwise to 7-amino-2-methyl-4-(4-propan-2-ylpiperazin-1-yl)-3H-isoindol-1-one (1.004 g, 3.48 mmol), in THF (30 mL) at room temperature under an atmosphere of nitrogen. The resulting suspension was stirred at room temperature for 30 minutes and then 4,6-dichloropyridine-3-carbonitrile (0.602 g, 3.48 mmol) was added portionwise and the mixture heated overnight at 60° C. The mixture was allowed to cool to room temperature and then diluted with EtOAc (50 mL). The mixture was washed sequentially with water (50 mL), a saturated solution of NaHCO3 (50 mL), water (25 mL) and finally with a saturated solution of NaCl (20 mL). The mixture was filtered and the organic layer separated, dried over Na2SO4 and then evaporated. The residue was triturated in Et2O and MeOH and the mixture filtered. The filtrate was evaporated and the residue purified by chromatography on silica, eluting with a gradient of 5-10% MeOH in CH2Cl2. Fractions containing product were combined and evaporated to leave 6-chloro-[[2-methyl-3-oxo-7-(4-propan-2-ylpiperazin-1-yl)-1H-isoindol-4-yl]amino]pyridine-3-carbonitrile (316 mg, 21% yield); 1H NMR spectrum: (300 MHz, DMSO) δ 1.02 (6H, d), 2.60 (4H, t), 2.70 (1H, t), 3.02-3.08 (7H, m), 4.51 (2H, s), 7.04 (1H, d), 7.15 (1H, dd), 7.44 (1H, dd), 8.53 (1H, d), 9.68 (1H, s); Mass spectrum: m/z (ESI+) (M+H)+=425.30.

후처리

  1. temperaturethe mixture heated overnight at 60° C
  2. temperatureto cool to room temperature
  3. washThe mixture was washed sequentially with water (50 mL)
  4. filtrationThe mixture was filtered
  5. customthe organic layer separated
  6. dry with materialdried over Na2SO4
  7. customevaporated
  8. customThe residue was triturated in Et2O
  9. filtrationMeOH and the mixture filtered
  10. customThe filtrate was evaporated
  11. customthe residue purified by chromatography on silica
  12. washeluting with a gradient of 5-10% MeOH in CH2Cl2
  13. additionFractions containing product
  14. customevaporated

출처 및 근거

ORD 기록
ord-97e3c31a00e14b36912fb4b24105ab16
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08569298B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트