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

Ammonium Chloride → (racemic) N-(4-(4-chloro-2-hydroxybutoxy)-5-cyanopyridin-2-yl)-7-formyl-6-(hydroxymethyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxamide

HRID 1778086
노트
인쇄 미리보기

반응식

HRID 1778086 반응식
[Si]([O:8][CH2:9][C:10]1[CH:11]=[C:12]2[C:17](=[N:18][C:19]=1[CH:20]([O:23]C)OC)[N:16]([C:25]([O:27]C1C=CC=CC=1)=O)[CH2:15][CH2:14][CH2:13]2)(C(C)(C)C)(C)C.[NH2:34][C:35]1[CH:42]=[C:41]([O:43][CH2:44][CH:45]2[CH2:48][CH2:47][O:46]2)[C:38]([C:39]#[N:40])=[CH:37][N:36]=1.[Li+].C[Si]([N-][Si](C)(C)C)(C)C.[NH4+].[Cl-:60]>C1COCC1>[Cl:60][CH2:47][CH2:48][CH:45]([OH:46])[CH2:44][O:43][C:41]1[C:38]([C:39]#[N:40])=[CH:37][N:36]=[C:35]([NH:34][C:25]([N:16]2[C:17]3[C:12](=[CH:11][C:10]([CH2:9][OH:8])=[C:19]([CH:20]=[O:23])[N:18]=3)[CH2:13][CH2:14][CH2:15]2)=[O:27])[CH:42]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 2733832Lithium hexamethyldisilazaneHCID 1180363096-Amino-4-(oxetan-2-ylmethoxy)nicotinonitrile2회HCID 131734775phenyl 6-(((tert-butyldimethylsilyl)oxy)methyl)-7-(dimethoxymethyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxylate2회

생성물 1

HCID 118036772
(racemic) N-(4-(4-chloro-2-hydroxybutoxy)-5-cyanopyridin-2-yl)-7-formyl-6-(hydroxymethyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
-78 °C

실험 절차

Phenyl 6-(((tert-butyldimethylsilyl)oxy)methyl)-7-(dimethoxymethyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxylate (intermediate 38, 105 mg, 0.222 mmol) and 6-amino-4-(oxetan-2-ylmethoxy)nicotinonitrile (intermediate 34A, 54.7 mg, 0.267 mmol) were dissolved in THF (2 ml) under argon. The resulting solution was cooled to −78° C. and treated slowly with LHMDS (1 M in THF, 0.489 ml, 0.498 mmol). The reaction mixture was stirred at −78° C. for 45 min and then slowly warmed up to room temperature. The reaction mixture was poured into sat. aq. NH4Cl and extracted twice with DCM. The organic phase was then dried over Na2SO4, filtered and evaporated. The crude material was purified by preparative supercritical fluid chromatography (SFC 1, NH2 column). The 6-(((tert-butyldimethylsilyl)oxy)methyl)-N-(5-cyano-4-(oxetan-2-ylmethoxy)pyridin-2-yl)-7-(dimethoxymethyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxamide containing fractions were concentrated and then dissolved in THF (2 ml) and water (2 ml) and treated with conc. HCl (0.39 ml). The reaction mixture was stirred 16 h at room temperature. The reaction mixture was quenched with aq. sat. NaHCO3 and extracted 3× with DCM. The org layer was dried over Na2SO4, filtered and concentrated under vacuum. The crude material was treated with a small quantity of DCM and then the product was precipitated by addition of heptanes. The solid was collected by centrifugation and dried under vacuum to obtain the title compound as a white solid.

후처리

  1. temperatureslowly warmed up to room temperature
  2. extractionextracted twice with DCM
  3. dry with materialThe organic phase was then dried over Na2SO4
  4. filtrationfiltered
  5. customevaporated
  6. customThe crude material was purified by preparative supercritical fluid chromatography (SFC 1, NH2 column)
  7. concentrationThe 6-(((tert-butyldimethylsilyl)oxy)methyl)-N-(5-cyano-4-(oxetan-2-ylmethoxy)pyridin-2-yl)-7-(dimethoxymethyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxamide containing fractions were concentrated
  8. dissolutiondissolved in THF (2 ml)
  9. additionwater (2 ml) and treated with conc. HCl (0.39 ml)
  10. stirringThe reaction mixture was stirred 16 h at room temperature
  11. customThe reaction mixture was quenched with aq. sat. NaHCO3
  12. extractionextracted 3× with DCM
  13. dry with materialThe org layer was dried over Na2SO4
  14. filtrationfiltered
  15. concentrationconcentrated under vacuum
  16. additionThe crude material was treated with a small quantity of DCM
  17. customthe product was precipitated by addition of heptanes
  18. customThe solid was collected by centrifugation
  19. customdried under vacuum

출처 및 근거

ORD 기록
ord-6c413dbe06b64c85b7f57c515eb5c2e9
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09266883B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트