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Hydrazine → HCID 10240087, 화합물

HRID 1862010
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HRID 1862010 반응식
C1(=O)[N:5]([CH2:6][CH2:7][O:8][C@@H:9]2[C@H:13]([OH:14])[C@@H:12]([CH2:15][O:16][C:17]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)([C:26]3[CH:31]=[CH:30][C:29]([O:32][CH3:33])=[CH:28][CH:27]=3)[C:18]3[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=3)[O:11][C@H:10]2[N:40]2[CH:47]=[C:46]([CH3:48])[C:44](=[O:45])[NH:43][C:41]2=[O:42])C(=O)C2=CC=CC=C12.NN>CO>[CH3:7][OH:8].[OH-:8].[NH4+:5].[NH2:5][CH2:6][CH2:7][O:8][C@@H:9]1[C@H:13]([OH:14])[C@@H:12]([CH2:15][O:16][C:17]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)([C:18]2[CH:19]=[CH:20][C:21]([O:24][CH3:25])=[CH:22][CH:23]=2)[C:26]2[CH:31]=[CH:30][C:29]([O:32][CH3:33])=[CH:28][CH:27]=2)[O:11][C@H:10]1[N:40]1[CH:47]=[C:46]([CH3:48])[C:44](=[O:45])[NH:43][C:41]1=[O:42]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 9321HydrazineHCID 10628754HCID 10628754, 화합물

생성물 2

HCID 10240087HCID 10240087, 화합물수율 212.5%HCID 21894508Ammonium hydroxide methanol

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2′-O-Phthalimidoethyl-5′-O-DMT-5-methyluridine (3, 21.1 g, 0.029 mol) was dissolved in methanol (500 mL). Anhydrous hydrazine (4.9 mL, 0.15 mol) was added and the solution was heated to reflux. TLC after 3 h indicated a complete reaction. The residue was purified by chromatography on silica gel using methanol and then methanol-ammonium hydroxide (98:2) to give 4 (12.4 g, 70%). The material was completely soluble in methylene chloride and traces of silica from leaching of the column were removed by filtration at this stage and reevaporating the solution.

후처리

  1. temperaturethe solution was heated to reflux
  2. customa complete reaction
  3. customThe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-dad4269e502448afb440b7d019eabc62
출처 데이터셋
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06534639B1

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