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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 47453787, 화합물 → HCID 59596398, 화합물

HRID 2264606
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HRID 2264606 반응식
Cl[C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:10]=[C:11]3[C:16](=[CH:17][CH:18]=2)[N:15]=[CH:14][CH:13]=[CH:12]3)[N:5]=[C:4]([NH2:19])[N:3]=1>C1COCC1.[Pd]>[NH:15]1[C:16]2[C:11](=[CH:10][C:9]([O:8][C:6]3[CH:7]=[CH:2][N:3]=[C:4]([NH2:19])[N:5]=3)=[CH:18][CH:17]=2)[CH2:12][CH2:13][CH2:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 47453787HCID 47453787, 화합물

생성물 1

HCID 59596398HCID 59596398, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 5.4 g (0.02 mol) 4-chloro-6-(quinolin-6-yloxy)-pyrimidin-2-ylamine in 600 mL of THF is hydrogenated during 21 h in the presence of 1.2 g Pd/C (10% Engelhard 4505). Then the catalyst is filtered off and the filtrate concentrated in vacuuo. The residue is partitioned between ethyl acetate and conc. sodium bicarbonate solution and the organic layer washed with brine, dried and evaporated. The crude product is purified by flash-chromatography on silica gel using dichloromethane/methanol 95:5 as eluent. Fractions with pure compound are pooled and evaporated. The crystalline material is triturated with ether, filtered and dried to give the title compound: m.p. 180-182° C.; MS: [M+1]+=243; TLC (dichloromethane/methanol 95:5): Rf=0.4.

후처리

  1. filtrationThen the catalyst is filtered off
  2. concentrationthe filtrate concentrated in vacuuo
  3. customThe residue is partitioned between ethyl acetate and conc. sodium bicarbonate solution
  4. washthe organic layer washed with brine
  5. customdried
  6. customevaporated
  7. customThe crude product is purified by flash-chromatography on silica gel
  8. customevaporated
  9. customThe crystalline material is triturated with ether
  10. filtrationfiltered
  11. customdried

출처 및 근거

ORD 기록
ord-256ba812e35746868ea1714b7eca2bcd
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07855215B2

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