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Water → HCID 69416361, 화합물

HRID 1270162
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HRID 1270162 반응식
Br[C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([NH:17][CH:18]([CH3:20])[CH3:19])[C:8]3[N:9]2[C:12]([O:15]C)=[N:13][N:14]=3)=[CH:4][CH:3]=1.[C:21]1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(N(CC)CC)C.[CH3:57][OH:58].CS(C)=O.[OH2:63]>C(Cl)Cl>[CH3:57][O:58][C:21]([C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([NH:17][CH:18]([CH3:20])[CH3:19])[C:8]3[N:9]2[C:12](=[O:15])[NH:13][N:14]=3)=[CH:4][CH:3]=1)=[O:63]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 962WaterHCID 8471TriethylamineHCID 812191,3-Bis(diphenylphosphino)propaneHCID 18449223HCID 18449223, 화합물HCID 22036561Dimethyl sulfoxide methanol

생성물 1

HCID 69416361HCID 69416361, 화합물

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

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온도
75 °C

실험 절차

A solution of 2.0 g of (8-bromo-1-methoxy-[1,2,4]triazolo[4,3-a]quinoxalin-4-yl)-isopropyl-amine, 0.54 g of Pd(II)acetate, 0.66 g of 1,3-bis-(diphenylphosphino)propane, and triethylamine (21 mL) in a 1.1/1.0 mixture of MeOH/DMSO was agitated under an atmosphere of CO (45 psi) at 75° C. for 96 hrs. After cooling to 23° C., the solution was diluted with water and methylene chloride and the resulting mixture filtered through diatomaceous earth. The filtrate was concentrated and the residue was dissolved in methylene chloride and washed with brine (2×). The title compound precipitated from the organic layer upon standing and was isolated by filtration. MS (M+H)+=302.3.

후처리

  1. temperatureAfter cooling to 23° C.
  2. filtrationthe resulting mixture filtered through diatomaceous earth
  3. concentrationThe filtrate was concentrated
  4. dissolutionthe residue was dissolved in methylene chloride
  5. washwashed with brine (2×)
  6. customThe title compound precipitated from the organic layer
  7. customwas isolated by filtration

출처 및 근거

ORD 기록
ord-cd5b2c331dfc436d81f548adeab09221
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07202245B2

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