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Iodine → HCID 117709797, 화합물

HRID 2274166
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HRID 2274166 반응식
C([O:8][C:9]1[N:14]=[C:13]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:12]=[C:11]([O:23]CC2C=CC=CC=2)[N:10]=1)C1C=CC=CC=1.II.S([O-])([O-])(=O)=S.[Na+].[Na+].[C:40]1([CH3:46])[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1>>[CH2:46]([N:14]1[C:13]([O:15][CH2:16][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)=[N:12][C:11](=[O:23])[N:10]([CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:9]1=[O:8])[C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 807IodineHCID 1140TolueneHCID 24477Sodium ThiosulfateHCID 2252572,4,6-tris(benzyloxy)-1,3,5-triazine

생성물 1

HCID 117709797HCID 117709797, 화합물수율 21%

실험 절차

Furthermore, a synthesis method of the hydroxy group-protecting agent 5 will be explained. To a 10 mL eggplant flask, 599.2 mg (1.50 m mol) of 2,4,6-tribenzyloxy-1,3,5-triazine, 5.00 mL of toluene and 38.8 mg (030 m mol) of iodine were added, heat-perfused, and reacted for 31 hours. After the reaction, 5 mL of an aqueous solution of saturated sodium thiosulfate was added, which was washed with 5 mL of 1 N sodium bicarbonate water, 5 mL of 1 N hydrochloric acid, 5 mL of water and 5 mL of saturated salt water. A resulting organic phase was dried by magnesium sulfate, from which the solvent was distilled away, and the residue was isolated and purified by silica-gel chromatography to obtain 126.2 mg of 1,3-dibenzyl-6-(benzyloxy)-1,3,5-triazine-2,4(1H,3H)-dione (yield: 21%).

후처리

  1. customheat-perfused, and reacted for 31 hours
  2. additionwas added
  3. washwhich was washed with 5 mL of 1 N sodium bicarbonate water, 5 mL of 1 N hydrochloric acid, 5 mL of water and 5 mL of saturated salt water
  4. dry with materialA resulting organic phase was dried by magnesium sulfate, from which the solvent
  5. distillationwas distilled away
  6. customthe residue was isolated
  7. custompurified by silica-gel chromatography

출처 및 근거

ORD 기록
ord-9e0afbaf25ec4d63ab680b7711a075e4
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09126954B2

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