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

Water → HCID 66637332, 화합물

HRID 1094637
노트
인쇄 미리보기

반응식

HRID 1094637 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH:9]([NH:11][S:12]([C:14]([CH3:17])([CH3:16])[CH3:15])=[O:13])[CH3:10])[CH:5]=[CH:6][C:7]=1[NH2:8].C1N=CN([C:23](N2C=NC=C2)=[O:24])C=1.O>C1COCC1.C(Cl)Cl>[CH3:17][C:14]([S:12]([NH:11][CH:9]([C:4]1[CH:5]=[CH:6][C:7]2[NH:8][C:23](=[O:24])[NH:1][C:2]=2[CH:3]=1)[CH3:10])=[O:13])([CH3:16])[CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 682631,1'-CarbonyldiimidazoleHCID 66637050HCID 66637050, 화합물

생성물 1

HCID 66637332HCID 66637332, 화합물수율 65%

시약·촉매·용매 1

HCID 21919333Tetrahydrofurane dichloromethane용매

실험 절차

A mixture of N-[1-(3,4-diaminophenyl)ethyl]-2-methylpropane-2-sulfinamide and CDI (569 mg, 3.51 mmol) in THF-DCM (10 ml-10 ml) was refluxed for 6 hours. After cooling to the room temperture, water (10 mL) was added to the mixture. The mixture was extracted with EtOAc (150 ml) and organic layer was washed with brine (30 ml), dried over sodium sulfate and concentrated. The residue was recrystallized from EtOAc to afford 430 mg (65%) of the title compound as a pale brown solid. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.11 (9H, s), 1.38 (3H, d, J=7.3 Hz), 4.37-4.28 (1H, m), 5.53 (1H, d, J=6.6 Hz), 6.84 (1H, d, J=7.3 Hz), 6.93 (1H, d, J=8.1 Hz), 6.99 (1H, s), 10.54 (1H, br.s), 10.60 (1H, br.s). MS (ESI) m/z 282 (M+H)+, 280 (M−H)−.

후처리

  1. temperaturewas refluxed for 6 hours
  2. additionwas added to the mixture
  3. extractionThe mixture was extracted with EtOAc (150 ml) and organic layer
  4. washwas washed with brine (30 ml)
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue was recrystallized from EtOAc

출처 및 근거

ORD 기록
ord-1456908fa4c441c7b3bb17738d4d0a93
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08134004B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트