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Triphosgene → 5,6-Dimethoxyisatoic anhydride

HRID 525956
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HRID 525956 반응식
[C:1](=O)(OC(Cl)(Cl)Cl)[O:2]C(Cl)(Cl)Cl.Cl.[NH2:14][C:15]1[C:20]([C:21]([OH:23])=[O:22])=[C:19]([O:24][CH3:25])[C:18]([O:26][CH3:27])=[CH:17][CH:16]=1>O>[CH3:25][O:24][C:19]1[C:20]2[C:21](=[O:23])[O:22][C:1](=[O:2])[NH:14][C:15]=2[CH:16]=[CH:17][C:18]=1[O:26][CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 94429TriphosgeneHCID 1317355906-Amino-2,3-dimethoxybenzoic acid hydrochloride

생성물 1

HCID 127623805,6-Dimethoxyisatoic anhydride수율 125%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Bis(trichloromethyl) carbonate (24.89 g, 84 mmol) was added into a solution of 6-amino-2,3-dimethoxybenzoic acid, Hydrochloride (28 g, 120 mmol) in Water (1.1 L). The mixture was stirred at r.t. over the weekend. The reaction mixture was filtered, the solid was collected and dried to afford 5,6-dimethoxy-1H-benzo[d][1,3]oxazine-2,4-dione (24 g, 105 mmol, 88% yield) as a light yellow solid. LCMS: (M+H)+: 223.9.

후처리

  1. filtrationThe reaction mixture was filtered
  2. customthe solid was collected
  3. customdried

출처 및 근거

ORD 기록
ord-44a2f8d6a6894dd7b82921f6a093038a
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09340556B2

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