Formamide → 4-Methoxyisoindoline-1,3-dione

HRID 41456

반응식

HRID 41456 반응식
[CH3:1][O:2][C:3]1[CH:13]=[CH:12][CH:11]=[C:5]2[C:6]([O:8][C:9](=O)[C:4]=12)=[O:7].C([NH2:16])=O>O>[CH3:1][O:2][C:3]1[CH:13]=[CH:12][CH:11]=[C:5]2[C:6]([NH:16][C:9](=[O:8])[C:4]=12)=[O:7]

참가 물질

4

반응물 2

HCID 713FormamideHCID 2911934-Methoxy-1,3-dihydro-2-benzofuran-1,3-dione

생성물 1

HCID 166382284-Methoxyisoindoline-1,3-dione수율 37%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 3-methoxyphthalic anhydride (24.0 g, 134.8 mmol) and formamide (120 ml) was stirred and held at 210° C. for 5 hours and was then allowed to cool to room temperature overnight. Water (100 ml) was added and the solid material filtered off under reduced pressure. The crude product was washed sequentially with 50% aqueous acetone (50 ml) and diethyl ether (200 ml) and sucked dry under reduced pressure to afford 3-methoxyphthalimide (8.95 g, 37%) as an off-white solid. 1H NMR (DMSO-d6) 11.08 (1H, br s), 7.78 (1H, dd), 7.45 (1H, d), 7.36 (1H, d), 3.93 (3H, s). MS: [M+H]+ 178.

후처리

  1. filtrationthe solid material filtered off under reduced pressure
  2. washThe crude product was washed sequentially with 50% aqueous acetone (50 ml) and diethyl ether (200 ml)
  3. customsucked dry under reduced pressure

출처 및 근거

ORD 기록
ord-ded08a33f7ef4150b3184e5faa2faedc
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530469B2

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