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

Hydrochloric Acid → HCID 21949958, 화합물

HRID 2215759
노트
인쇄 미리보기

반응식

HRID 2215759 반응식
CC([O-])(C)C.[K+].C1COCC1.[NH:12]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[C:14]([CH2:21][C:22]([NH2:24])=[O:23])=[CH:13]1.C[O:26][C:27](=O)[C:28]([C:30]1[CH:31]=[CH:32][CH:33]=[C:34]2[C:38]=1[N:37]([CH2:39][CH3:40])[CH:36]=[CH:35]2)=O.Cl>CN(C=O)C.CCOC(C)=O>[NH:12]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[C:14]([C:21]2[C:22](=[O:23])[NH:24][C:27](=[O:26])[C:28]=2[C:30]2[CH:31]=[CH:32][CH:33]=[C:34]3[C:38]=2[N:37]([CH2:39][CH3:40])[CH:36]=[CH:35]3)=[CH:13]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 397Indole-3-acetamideHCID 8028TetrahydrofuranHCID 23665647Potassium tert-butoxideHCID 69642170HCID 69642170, 화합물

생성물 1

HCID 21949958HCID 21949958, 화합물수율 38.6%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
50 °C

실험 절차

A 1.0 M solution of KOtBu in THF (6 mL, 6 mmol) was added to a solution of 2-(1H-indol-3-yl)-acetamide (478 mg, 2.75 mmol) and (1-ethyl-1H-indol-7-yl)-oxo-acetic acid methyl ester (635 mg, 2.75 mmol) in DMF (20 mL). The deep red-orange solution was stirred 12 h at 50° C., allowed to cool, and 1N HCl added. The orange mixture was poured into EtOAc, and the EtOAc layer was separated and washed with 1N HCl, water, saturated NaHCO3 and brine, dried (MgSO4), filtered, and concentrated onto SiO2. Flash chromatography (1:1 EtOAc:hexanes) followed by precipitation from hot methanol afforded the title compound (377 mg, 37%) as a orange-red solid. Heating under vacuum at 70° C. afforded material which was used without further purification. 1H NMR (400 MHz, DMSO-d6) 11.83 (br s, 1H), 11.13 (s, 1H), 7.94 (d, J=3 Hz, 1H), 7.61 (dd, J=8, 1.5 Hz, 1H), 7.3 (m, 2H), 6.93–7.0 (m, 3H), 6.48 (m, 3H), 6.48 (m, 2H), 6.3 (d, J=7 Hz, 1H), 4.0 (m, 2H), 1.06 (t, J=5 Hz, 3H). MS (electrospray, m/z) 354 (M−−1).

후처리

  1. temperatureto cool
  2. customthe EtOAc layer was separated
  3. washwashed with 1N HCl, water, saturated NaHCO3 and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated onto SiO2
  7. customFlash chromatography (1:1 EtOAc:hexanes) followed by precipitation from hot methanol

출처 및 근거

ORD 기록
ord-c4d714957b604b348e1f07749615d5e3
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07109229B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트