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Sodium Iodide → HCID 54389470, 화합물

HRID 356576
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HRID 356576 반응식
[OH:1][C:2]1[CH:3]=[CH:4][C:5]([N+:12]([O-:14])=[O:13])=[C:6]([CH:8]([OH:11])[CH:9]=[CH2:10])[CH:7]=1.[I-].[Na+].C(=O)([O-])[O-].[K+].[K+].S(C1C=CC(C)=CC=1)(O[CH2:27][CH2:28][CH2:29][NH:30][C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])(=O)=O>CN(C=O)C.C(OCC)(=O)C>[C:34]([O:33][C:31]([NH:30][CH2:29][CH2:28][CH2:27][O:1][C:2]1[CH:3]=[CH:4][C:5]([N+:12]([O-:14])=[O:13])=[C:6]([CH:8]([OH:11])[CH:9]=[CH2:10])[CH:7]=1)=[O:32])([CH3:37])([CH3:36])[CH3:35]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 131203023-((Tert-butoxycarbonyl)amino)propyl 4-methylbenzenesulfonateHCID 22061198HCID 22061198, 화합물

생성물 1

HCID 54389470HCID 54389470, 화합물수율 98%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

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온도
50 °C

실험 절차

1-(5'-Hydroxy-2'-nitrophenyl)-2-propen-1-ol (2.0 g) is dissolved in dry DMF (100 ml) and thereto are added sodium iodide (1 equivalent), potassium carbonate and 3-t-butoxycarbonylaminopropyl tosylate (1.5 equivalent). The mixture is stirred at 50° C. for 6 hours, and thereto is added ethyl acetate. The mixture is washed with a saturated sodium chloride solution and dried over sodium sulfate. The residue is purified by silica gel column chromatography to give 1-[5'-(3"-t-butoxycarbonylaminopropyloxy)-2'-nitrophenyl]-2-propen-1-ol (3.53 g) as a pale brown caramel.

후처리

  1. washThe mixture is washed with a saturated sodium chloride solution
  2. dry with materialdried over sodium sulfate
  3. customThe residue is purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-b5ea5783f30b41f8a49fd844e11c69ee
출처 데이터셋
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05837673

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