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

Water → HCID 178494819, 화합물

HRID 1453544
노트
인쇄 미리보기

반응식

HRID 1453544 반응식
[K].C[Si]([N-][Si](C)(C)C)(C)C.[Cl-].[CH3:12][O:13][CH2:14][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Br:34][C:35]1[N:39](CC#CC)[C:38]([C:44]([O:46][CH3:47])=[O:45])=[C:37]([CH:48]=O)[N:36]=1.O>C1(C)C=CC=CC=1.O1CCCC1>[Br:34][C:35]1[NH:39][C:38]([C:44]([O:46][CH3:47])=[O:45])=[C:37](/[CH:48]=[CH:12]/[O:13][CH3:14])[N:36]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 2723798Methoxymethyl-triphenylphosphonium chlorideHCID 21947682methyl 2-bromo-3-(2-butyn-1-yl)-5-formyl-3H-imidazole-4-carboxylateHCID 86585346Potassium bis-trimethylsilylamide

생성물 1

HCID 178494819HCID 178494819, 화합물

시약·촉매·용매 2

HCID 1140
Toluene
용매
HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
-70 °C

실험 절차

Under an argon atmosphere 38 ml of a 0.5 M solution of potassium-bis(trimethylsilyl)amide in toluene are added dropwise to an ice-cooled solution of 6.64 g methoxymethyltriphenyl phosphonium chloride in 140 ml of tetrahydrofuran over 10 min. The reaction mixture is stirred for a further 15 min in the ice bath and then cooled to −70° C. Then a solution of 4.41 g methyl 2-bromo-3-(2-butyn-1-yl)-5-formyl-3H-imidazole-4-carboxylate in 40 ml of tetrahydrofuran is added dropwise over 30 min. After a further 45 min stirring at −70° C. the solution is heated to ambient temperature and stirred for another 1 h at this temperature. Then water is added to the reaction solution and this is extracted with ethyl acetate. The organic extracts are dried over sodium sulphate, the solvent is removed and the residue is chromatographed through silica gel (cyclohexane/ethyl acetate 9:1->7:3).

후처리

  1. temperatureis heated to ambient temperature
  2. stirringstirred for another 1 h at this temperature
  3. extractionthis is extracted with ethyl acetate
  4. dry with materialThe organic extracts are dried over sodium sulphate
  5. customthe solvent is removed
  6. customthe residue is chromatographed through silica gel (cyclohexane/ethyl acetate 9:1->7:3)

출처 및 근거

ORD 기록
ord-af2ba0d1391f4d08be55d06190a9ce18
출처 데이터셋
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07476671B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트