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

Diethyl Oxalate → Ethyl [2-({7-(benzyloxy)-5-[4-(methylsulfonyl)phenoxy]-1H-indol-2-yl}carbonyl)hydrazino](oxo)acetate

HRID 1188891
노트
인쇄 미리보기

반응식

HRID 1188891 반응식
O.NN.[C:4]([O:11][CH2:12][CH3:13])(=[O:10])[C:5]([O:7]CC)=O.[CH2:14]([O:21][C:22]1[CH:23]=[C:24]([O:34][C:35]2[CH:40]=[CH:39][C:38]([S:41]([CH3:44])(=[O:43])=[O:42])=[CH:37][CH:36]=2)[CH:25]=[C:26]2[C:30]=1[NH:29][C:28]([C:31](O)=[O:32])=[CH:27]2)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.Cl.CN(C)CCCN=C=NCC.O[N:58]1C2C=CC=CC=2N=[N:59]1>C(O)C.CCCCCC.C(OCC)(=O)C.O.CN(C)C=O>[CH2:14]([O:21][C:22]1[CH:23]=[C:24]([O:34][C:35]2[CH:36]=[CH:37][C:38]([S:41]([CH3:44])(=[O:42])=[O:43])=[CH:39][CH:40]=2)[CH:25]=[C:26]2[C:30]=1[NH:29][C:28]([C:31]([NH:58][NH:59][C:5](=[O:7])[C:4]([O:11][CH2:12][CH3:13])=[O:10])=[O:32])=[CH:27]2)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 5

HCID 7268Diethyl OxalateHCID 24654Hydrazine hydrate (1:1)HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 668975467-(Benzyloxy)-5-[4-(methylsulfonyl)phenoxy]-1H-indole-2-carboxylic acid

생성물 1

HCID 66897270
Ethyl [2-({7-(benzyloxy)-5-[4-(methylsulfonyl)phenoxy]-1H-indol-2-yl}carbonyl)hydrazino](oxo)acetate
수율 83%

시약·촉매·용매 5

HCID 702Ethanol용매2회HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8058Hexane용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of hydrazine monohydrate (0.1 mL) in ethanol (2 mL) was added dropwise to a solution of diethyl oxalate (0.3 mL) in ethanol (2 mL) under ice-cooling. The reaction mixture was concentrated under reduced pressure to give a white solid. A mixture of 7-(benzyloxy)-5-[4-(methylsulfonyl)phenoxy]-1H-indole-2-carboxylic acid (450 mg), 1-[3-(dimethylamino)propyl-3-ethylcarbodiimide hydrochloride (403 mg), 1-hydroxybenzotriazole (284 mg) and N,N-dimethylformamide (20 mL) was stirred at room temperature for 30 min, the previous-obtained white solid was added, and the mixture was stirred at room temperature for 2 hr. Water was added to the reaction solution, and the mixture was subjected to extraction with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, filtrated, and concentrated under reduced pressure. The obtained crude product was subjected to silica gel column chromatography (ethyl acetate:hexane=20:80-90:10, volume ratio) to give the title compound (420 mg, yield 83%) as an orange oil. MS 552 (MH+).

후처리

  1. temperaturecooling
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customto give a white solid
  4. additionthe previous-obtained white solid was added
  5. stirringthe mixture was stirred at room temperature for 2 hr
  6. extractionthe mixture was subjected to extraction with ethyl acetate
  7. washThe organic layer was washed with saturated brine
  8. dry with materialdried over magnesium sulfate
  9. filtrationfiltrated
  10. concentrationconcentrated under reduced pressure
  11. customThe obtained crude product

출처 및 근거

ORD 기록
ord-2101a507ae0c47ba971d0f4dd294fd04
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08673942B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트