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

1,2-Dichloroethane → HCID 68469439, 화합물

HRID 506784
노트
인쇄 미리보기

반응식

HRID 506784 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[N:8]([S:24]([C:27]3[CH:32]=[CH:31][C:30]([CH3:33])=[CH:29][CH:28]=3)(=[O:26])=[O:25])[C:9]([C:11]3[C:15]4=[N:16][C:17]([O:22][CH3:23])=[C:18]([O:20][CH3:21])[CH:19]=[C:14]4[NH:13][CH:12]=3)=[CH:10][C:3]=12.[OH-].[Na+].[Cl:36][CH2:37][CH2:38]Cl>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[Cl:36][CH2:37][CH2:38][N:13]1[C:14]2[C:15](=[N:16][C:17]([O:22][CH3:23])=[C:18]([O:20][CH3:21])[CH:19]=2)[C:11]([C:9]2[N:8]([S:24]([C:27]3[CH:32]=[CH:31][C:30]([CH3:33])=[CH:29][CH:28]=3)(=[O:25])=[O:26])[C:4]3=[N:5][CH:6]=[CH:7][C:2]([Cl:1])=[C:3]3[CH:10]=2)=[CH:12]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 111,2-DichloroethaneHCID 14798Sodium HydroxideHCID 68467297HCID 68467297, 화합물

생성물 1

HCID 68469439HCID 68469439, 화합물수율 54%

시약·촉매·용매 1

HCID 74236Tetrabutylammonium Bromide촉매

반응 조건

온도
50 °C

실험 절차

Heat a mixture of bisazaindole 28 (180 mg, 0.373 mmol), 1,2-dichloroethane (2.0 mL), 9N NaOH (2.0 mL) and tetrabutylammonium bromide (16 mg), with stirring, at 50° C. for 16 h. Then leave the reaction medium to cool to room temperature, extract it with CH2Cl2 (3×), dry (Na2SO4) and concentrate under vacuum. Purification on SiO2 by flash chromatography gives 31 (110 mg, 54%) as a yellow solid: 1H NMR (CDCl3) δ 8.40 (d, 1H, J=5.4 Hz), 7.76 (d, 1H, J=5.2 Hz), 7.70 (d, 2H, J=8.4 Hz), 7.59 (s, 1H), 7.15 (m, 2H), 7.06 (d, 2H, J=8.4 Hz), 7.02 (s, 1H), 4.51 (t, 2H, J=6.4 Hz), 4.06 (s, 3H), 4.00 (s, 3H), 3.90 (t, 2H, J=6.4 Hz), 2.30 (s, 3H), TLC (EtOAc at 40%/heptane) Rf=0.20.

후처리

  1. temperatureHeat
  2. customThen leave
  3. customthe reaction medium
  4. temperatureto cool to room temperature
  5. extractionextract it with CH2Cl2 (3×)
  6. dry with materialdry (Na2SO4)
  7. concentrationconcentrate under vacuum
  8. customPurification on SiO2 by flash chromatography

출처 및 근거

ORD 기록
ord-4ee1d9db0cbf440aa34fa9b337f9a88c
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07786114B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트