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Triphosgene → HCID 86717347, 화합물

HRID 527145
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HRID 527145 반응식
[NH2:1][C:2]1([C:13]2[CH:18]=[CH:17][C:16]([CH:19]([CH3:21])[CH3:20])=[CH:15][C:14]=2[O:22][CH3:23])[C:10](=[O:11])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]1=[O:12].Cl[C:25](Cl)([O:27]C(=O)OC(Cl)(Cl)Cl)Cl.Cl.[CH3:37][O:38][NH2:39]>C1COCC1>[CH:19]([C:16]1[CH:17]=[CH:18][C:13]([C:2]2([NH:1][C:25]([NH:39][O:38][CH3:37])=[O:27])[C:10](=[O:11])[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[C:3]2=[O:12])=[C:14]([O:22][CH3:23])[CH:15]=1)([CH3:21])[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 94429TriphosgeneHCID 521874O-Methylhydroxylamine hydrochlorideHCID 86717345HCID 86717345, 화합물

생성물 1

HCID 86717347HCID 86717347, 화합물수율 69%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 2-amino-2-(4-isopropyl-2-methoxyphenyl)-2H-inden-1,3-dione (0.50 g, 1.61 mmol) in anhydrous THF (20 ml) was added triphosgene (0.528 g, 1.77 mmol) and stirred for 15 min. The reaction mixture was concentrated and was dissolved in anhydrous THF (20 ml) and was added O-methyl-hydroxylamine hydrochloride (0.28 g, 4.04 mmol) was stirred for 2 hrs at room temperature. The reaction mixture was oncentrated and was purified using silica gel column chromatography (1:1=ethylacetate:hexane) to afford the title compound (420 mg, 69%).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionwas dissolved in anhydrous THF (20 ml)
  3. stirringwas stirred for 2 hrs at room temperature
  4. customwas purified

출처 및 근거

ORD 기록
ord-4dbcf232a8d64c98933cb24e46e1c68d
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09346749B2

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