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

Sodium Iodide → 1-(Ethyloxycarbonyloxy)ethyl 5-(N-acetylamino)-3-(N-methylaminocarbonyl)-2,4,6-triiodobenzenecarboxylate

HRID 36783
노트
인쇄 미리보기

반응식

HRID 36783 반응식
[C:1](=[O:9])([O:6][CH2:7][CH3:8])[O:2][CH:3](Cl)[CH3:4].[C:10]([NH:13][C:14]1[C:15]([I:29])=[C:16]([C:25]([NH:27][CH3:28])=[O:26])[C:17]([I:24])=[C:18]([C:21]([O-:23])=[O:22])[C:19]=1[I:20])(=[O:12])[CH3:11].[K+].[I-].[Na+]>CN(C=O)C>[C:10]([NH:13][C:14]1[C:15]([I:29])=[C:16]([C:25]([NH:27][CH3:28])=[O:26])[C:17]([I:24])=[C:18]([C:21]([O:23][CH:3]([O:2][C:1]([O:6][CH2:7][CH3:8])=[O:9])[CH3:4])=[O:22])[C:19]=1[I:20])(=[O:12])[CH3:11]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 5238Sodium IodideHCID 162095Carbonic acid, 1-chloroethyl ethyl esterHCID 23692363potassium 5-(N-acetylamino)-3-(methylaminocarbonyl)-2,4,6-triiodobenzenecarboxylate

생성물 1

HCID 194227621-(Ethyloxycarbonyloxy)ethyl 5-(N-acetylamino)-3-(N-methylaminocarbonyl)-2,4,6-triiodobenzenecarboxylate

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

반응 조건

온도
50 °C

실험 절차

1-Chloroethyl ethyl carbonate (1.67 g, 11.0 mmol) was added dropwise at room temperature to a solution of potassium 5-(N-acetylamino)-3-(N-methylaminocarbonyl)-2,4,6-triiodobenzenecarboxylate (6.52 g, 10.0 mmol) and sodium iodide (150 mg, 1.0 mmol) in dry DMF (50 ml). After stirring at 50° C. for 24 hours the solvent was removed at reduced pressure. The residue was dissolved in chloroform and washed four times with a saturated sodium hydrogen carbonate solution and twice with water. After drying with magnesium sulfate and filtration, the solvent was removed at reduced pressure to give the title compound. Yield: (2.2 g, 38 %). Purity by HPLC: 98%. 1H-NMR (DMSO-d6 ): delta=1.24 (t, J=7 Hz, CH3 ); 1.63 (d, J=6 Hz, CH3); 2.03 (s, CH3CO); 2.75 (d, J=3 Hz, NCH3); 4.21 (q, J=7 Hz, CH2): 6.93 (q, J=6 Hz, CH); 8.4-8.7 (m, NHMe); 10.03 ppm (s, NHAc).

후처리

  1. customwas removed at reduced pressure
  2. dissolutionThe residue was dissolved in chloroform
  3. washwashed four times with a saturated sodium hydrogen carbonate solution
  4. dry with materialAfter drying with magnesium sulfate and filtration
  5. customthe solvent was removed at reduced pressure

출처 및 근거

ORD 기록
ord-91f97f67ff644647897a849387d38d85
출처 데이터셋
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05416223

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트