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

Water → HCID 66954001, 화합물

HRID 1619120
노트
인쇄 미리보기

반응식

HRID 1619120 반응식
[CH3:1][C:2](C)([O-])C.[K+].[Br:7][C:8]1[CH:9]=[C:10]2[NH:16][C:15](=[O:17])[CH2:14][C:11]2=[N:12][CH:13]=1.[C:18]([O:22]C)(=O)[CH:19]=[CH2:20].O>CS(C)=O.C(OCC)(=O)C>[Br:7][C:8]1[CH:9]=[C:10]2[NH:16][C:15](=[O:17])[C:14]3([CH2:20][CH2:19][C:18](=[O:22])[CH2:2][CH2:1]3)[C:11]2=[N:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 7294Methyl AcrylateHCID 23665647Potassium tert-butoxide2회HCID 469416416-Bromo-1,3-dihydro-2H-pyrrolo(3,2-b)pyridin-2-one

생성물 1

HCID 66954001HCID 66954001, 화합물수율 753%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide
용매
HCID 8857Ethyl Acetate용매

실험 절차

Potassium tert-butoxide (0.03 g, 0.27 mmol) was added to a suspension of 6-bromo-1H-pyrrolo[3,2-b]pyridin-2(3H)-one (preparation 30c, 0.87 g, 4.1 mmol) in dimethylsulphoxide (4 mL) and, after stirring for 10 minutes at room temperature, the mixture was heated to 40-45° C. and methyl acrylate (1.14 mL, 12.71 mmol) was added dropwise over 60 minutes. After the addition, the mixture was stirred for 2 hours and then further potassium tert-butoxide (1.4 g, 12.21 mmol) was added portionwise over 30 minutes keeping the temperature below 50° C. The mixture was then heated to 100° C. and stirred for 2 hours. Water (20 mL) was added and heating was continued at 85° C. for 2 hours and then the mixture was left to cool overnight. Ethyl acetate was added and the mixture was washed with water, brine, dried (MgSO4) and evaporated to give the title compound (0.60 g, 50%) as a white solid.

후처리

  1. temperaturethe mixture was heated to 40-45° C.
  2. additionAfter the addition
  3. stirringthe mixture was stirred for 2 hours
  4. customthe temperature below 50° C
  5. temperatureThe mixture was then heated to 100° C.
  6. stirringstirred for 2 hours
  7. temperatureheating
  8. waitwas continued at 85° C. for 2 hours
  9. waitthe mixture was left
  10. temperatureto cool overnight
  11. washthe mixture was washed with water, brine
  12. dry with materialdried (MgSO4)
  13. customevaporated

출처 및 근거

ORD 기록
ord-28a94945f4ac45ef8596cb806c5e5ab7
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772288B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트