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

1,1'-Carbonyldiimidazole → HCID 25138378, 화합물

HRID 1880617
노트
인쇄 미리보기

반응식

HRID 1880617 반응식
C1N=CN(C(N2C=NC=C2)=O)C=1.[F:13][C:14]([F:27])([F:26])[C:15]1[N:20]=[CH:19][C:18](/[CH:21]=[CH:22]/[C:23]([OH:25])=O)=[CH:17][CH:16]=1.C1C=CC2N(O)N=NC=2C=1.Br.[Cl:39][C:40]1[C:49]([OH:50])=[C:48]([OH:51])[C:47]([Cl:52])=[C:46]2[C:41]=1[CH2:42][CH2:43][NH:44][CH2:45]2>CCOC(C)=O.O>[Cl:39][C:40]1[C:49]([OH:50])=[C:48]([OH:51])[C:47]([Cl:52])=[C:46]2[C:41]=1[CH2:42][CH2:43][N:44]([C:23](=[O:25])/[CH:22]=[CH:21]/[C:18]1[CH:19]=[N:20][C:15]([C:14]([F:13])([F:27])[F:26])=[CH:16][CH:17]=1)[CH2:45]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 682631,1'-CarbonyldiimidazoleHCID 757711-HydroxybenzotriazoleHCID 5709645(2E)-3-[6-(Trifluoromethyl)pyridin-3-yl]prop-2-enoic acidHCID 685081725,8-Dichloro-1,2,3,4-tetrahydroisoquinoline-6,7-diol hydrobromide

생성물 1

HCID 25138378HCID 25138378, 화합물수율 55%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of CDI (83 mg, 0.51 mmol) in EtOAc (2 mL) was added (E)-3-(6-(trifluoromethyl)pyridin-3-yl)acrylic acid (100 mg, 0.46 mmol). The resulting mixture was heated at reflux for 1 h after which HOBt (35 mg, 0.23 mmol) and 5,8-dichloro-1,2,3,4-tetrahydroisoquinoline-6,7-diol hydro bromide (145 mg, 0.46 mmol) were added. Heating at reflux was continued for 3 h before the reaction mixture was allowed to cool to rt. It was then poured into water (15 mL) and the water-phase was extracted with EtOAc (3×15 mL). Combined organics were washed with water (10 mL) and brine (10 mL) and dried (MgSO4). After filtration and evaporation, the crude was purified by column chromatography (SiO2, EtOAc:petroleum ether 50:50) to give a bright yellow solid which was purified further by precipitating the product in EtOAc via addition of petroleum ether. After decantation of the solvent and drying, the title compound (110 mg, 0.25 mmol, 55%) was obtained as a light reddish solid.

후처리

  1. temperatureThe resulting mixture was heated
  2. additionwere added
  3. temperatureHeating
  4. temperatureat reflux
  5. extractionthe water-phase was extracted with EtOAc (3×15 mL)
  6. washCombined organics were washed with water (10 mL) and brine (10 mL)
  7. dry with materialdried (MgSO4)
  8. filtrationAfter filtration and evaporation
  9. customthe crude was purified by column chromatography (SiO2, EtOAc:petroleum ether 50:50)
  10. customto give a bright yellow solid which
  11. customwas purified further
  12. customby precipitating the product in EtOAc
  13. additionvia addition of petroleum ether
  14. customAfter decantation of the solvent and drying

출처 및 근거

ORD 기록
ord-eaf145bd000042eda80fcef18018cfc6
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318768B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트