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Acetic Acid → 1H-Isoindole-1,3(2H)-dione, 4-nitro-2-(3-pyridinylmethyl)-

HRID 1609583
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인쇄 미리보기

반응식

HRID 1609583 반응식
[N+:1]([C:4]1[CH:14]=[CH:13][CH:12]=[C:6]2[C:7]([O:9][C:10](=[O:11])[C:5]=12)=O)([O-:3])=[O:2].C(O)(=O)C.[NH2:19][CH2:20][C:21]1[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=1>C1(C)C=CC=CC=1>[N+:1]([C:4]1[CH:14]=[CH:13][CH:12]=[C:6]2[C:5]=1[C:10](=[O:11])[N:19]([CH2:20][C:21]1[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=1)[C:7]2=[O:9])([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 216313-Nitrophthalic anhydrideHCID 310183-Pyridinemethanamine

생성물 1

HCID 110005281H-Isoindole-1,3(2H)-dione, 4-nitro-2-(3-pyridinylmethyl)-수율 93.6%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a mixture of 15.0 g of 3-nitrophthalic acid anhydride, 233 ml of acetic acid and 80 ml of toluene was added 10.1 g of 3-aminomethylpyridine, and the resultant mixture was refluxed for 1.5 hours under heating. The reaction mixture was concentrated in vacuo, diluted with ethyl acetate, washed with 1N aqueous sodium hydroxide and water in order, dried over anhydrous magnesium sulfate and concentrated in vacuo to give 20.6 g of the titled compound.

후처리

  1. temperatureunder heating
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. additiondiluted with ethyl acetate
  4. washwashed with 1N aqueous sodium hydroxide and water in order
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-d8b0e9d58bd649efb6b6cdb05b3e4963
출처 데이터셋
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05401756

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