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

Sodium Carbonate → HCID 117993486, 화합물

HRID 922589
노트
인쇄 미리보기

반응식

HRID 922589 반응식
Cl[C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([C@@:10]2([CH3:16])[CH2:14][CH2:13][NH:12][C:11]2=[O:15])=[CH:4][CH:3]=1.[CH3:17][N:18]1[C:26]2[C:21](=[CH:22][C:23](B(O)O)=[CH:24][CH:25]=2)[CH:20]=[CH:19]1.C([O-])([O-])=O.[Na+].[Na+]>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].O1CCOCC1>[CH3:9][O:8][C:6]1[C:5]([C@@:10]2([CH3:16])[CH2:14][CH2:13][NH:12][C:11]2=[O:15])=[CH:4][CH:3]=[C:2]([C:23]2[CH:22]=[C:21]3[C:26](=[CH:25][CH:24]=2)[N:18]([CH3:17])[CH:19]=[CH:20]3)[N:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 27598671-Methyl-1H-indole-5-boronic acidHCID 117992994(R)-3-(6-chloro-2-methoxypyridin-3-yl)-3-methylpyrrolidin-2-one

생성물 1

HCID 117993486HCID 117993486, 화합물수율 99%

시약·촉매·용매 2

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매
HCID 312751,4-Dioxane용매

반응 조건

온도
110 °C

실험 절차

To a vial was added (R)-3-(6-chloro-2-methoxypyridin-3-yl)-3-methylpyrrolidin-2-one (56.6 mg, 0.24 mmol) which was evaporated with dioxane (2.0 mL). 1-methyl-1H-indol-5-ylboronic acid (63.4 mg, 0.36 mmol) was next added followed by Pd(dppf)Cl2 (7.5 mg, 0.01 mmol). The mixture was sealed and degassed with nitrogen. Degassed dioxane (1.9 mL) and degassed 2 M Na2CO3 (0.27 mL, 2.3 equiv) were then added to the solid mixture. The reaction was stirred for 16 h at 110° C. The reaction was concentrated and partitioned between EtOAc/10% (w/v) aq. Na2CO3. The organic layer was washed with brine, dried over Na2SO4, and concentrated to provide a crude brown glass. Purification by column chromatography (4 g RediSep Gold column) with a 40-100% EtOAc/heptane gradient provided the title compound (78 mg, 99%) as a pale yellow glass. 1H NMR (600 MHz, CDCl3) δ: 1.62 (s, 3H), 2.10 (ddd, 1H), 2.67-2.76 (m, 1H), 3.37-3.47 (m, 2H), 3.82 (s, 3H), 4.10-4.12 (m, 3H), 5.59 (br. s., 1H), 6.56 (d, 1H), 7.07 (d, 1H), 7.34-7.39 (m, 2H), 7.67 (d, 1H), 7.92-7.96 (m, 1H), 8.30 (s, 1H); MS (AP+)(M+H) 336. The absolute stereochemistry was obtained via X-ray crystallographic analysis of single crystals obtained via crystallization from a mixture of DCM and EtOH. FIG. 2 is an ORTEP drawing of (R)-3-(2-methoxy-6-(1-methyl-H-indol-5-yl)pyridin-3-yl)-3-methylpyrrolidin-2-one.

후처리

  1. customwas evaporated with dioxane (2.0 mL)
  2. additionnext added
  3. customThe mixture was sealed
  4. customdegassed with nitrogen
  5. additionwere then added to the solid mixture
  6. concentrationThe reaction was concentrated
  7. custompartitioned between EtOAc/10% (w/v) aq. Na2CO3
  8. washThe organic layer was washed with brine
  9. dry with materialdried over Na2SO4
  10. concentrationconcentrated
  11. customto provide a crude brown glass
  12. customPurification by column chromatography (4 g RediSep Gold column) with a 40-100% EtOAc/heptane gradient

출처 및 근거

ORD 기록
ord-2ceca911454f420b9589d2be75a8014e
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09278953B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트