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

p-Toluenesulfonic acid → HCID 67696440, 화합물

HRID 1609392
노트
인쇄 미리보기

반응식

HRID 1609392 반응식
[C:1](Cl)(=O)[C:2](Cl)=[O:3].[C:7]([O:10][CH2:11][CH:12]1[CH2:24][CH2:23][N:15]2[C:16]3[C:21]([CH:22]=[C:14]2[CH2:13]1)=[CH:20][CH:19]=[CH:18][CH:17]=3)(=[O:9])[CH3:8].C(N(CC)CC)C.Cl.[NH:33]1[C:41]2[C:36](=[CH:37][CH:38]=[CH:39][CH:40]=2)[C:35]([CH2:42][C:43](=[NH:48])[O:44]C(C)C)=[CH:34]1.C1(C)C=CC(S(O)(=O)=O)=CC=1>ClCCl.C1(C)C=CC=CC=1>[C:7]([O:10][CH2:11][CH:12]1[CH2:24][CH2:23][N:15]2[C:16]3[C:21]([C:22]([C:1]4[C:2](=[O:3])[NH:44][C:43](=[O:48])[C:42]=4[C:35]4[C:36]5[C:41](=[CH:40][CH:39]=[CH:38][CH:37]=5)[NH:33][CH:34]=4)=[C:14]2[CH2:13]1)=[CH:20][CH:19]=[CH:18][CH:17]=3)(=[O:9])[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 6101p-Toluenesulfonic acidHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 14954045HCID 14954045, 화합물HCID 20084644HCID 20084644, 화합물

생성물 1

HCID 67696440HCID 67696440, 화합물수율 38%

시약·촉매·용매 2

HCID 1140
Toluene
용매
HCID 6344Dichloromethane용매

실험 절차

165 mg (1.38 mmol) of oxalyl chloride were added to a stirred solution of 300 mg (1.24 mmol) of 8-acetoxymethyl-6,7,8,9-tetrahydropyrido[1,2-a]indole in 50 ml of dichloromethane at 0° C. The resulting solution was stirred for 15 minutes and the solvent was removed by evaporation. The residue was dissolved in 30 ml of toluene and added dropwise to a stirred solution of 496 mg (4.96 mmol) of triethylamine and mg (1.31 mmol) of isopropyl 3-indoleacetimidate hydrochloride in 20 ml of toluene. After 18 hours, 1.16 g (6.2 mmol) of p-toluenesulfonic acid were added and stirring was continued for 1 hour. The mixture was then partitioned between dichloromethane and water. The organic phase was dried over sodium sulfate and evaporated to dryness. The residue was purified by flash chromatography on silica gel using ethyl acetate/petroleum ether (1:1) for the elution to give 170 mg (38%) of 3-[8-(acetoxymethyl) -6,7,8,9-tetrahydropyrido[1,2-a]indol-10-yl]-4-[3-indolyl)-1H-pyrrole-2,5-dione in the form of an orange colored solid of melting point 264°-265° C.

후처리

  1. customthe solvent was removed by evaporation
  2. dissolutionThe residue was dissolved in 30 ml of toluene
  3. waitAfter 18 hours
  4. stirringstirring
  5. waitwas continued for 1 hour
  6. customThe mixture was then partitioned between dichloromethane and water
  7. dry with materialThe organic phase was dried over sodium sulfate
  8. customevaporated to dryness
  9. customThe residue was purified by flash chromatography on silica gel
  10. washfor the elution

출처 및 근거

ORD 기록
ord-1f6073b1febc44cd89158fd842ee643b
출처 데이터셋
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05399712

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트