2,5-Dimethoxytetrahydrofuran → N-(7-Nitro-2,4-dioxo-6-pyrrol-1-yl-1,4-dihydro-2H-quinazolin-3-yl)-methanesulfonamide

HRID 2069198노트

반응식

HRID 2069198 반응식
[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N+:12]([O-:14])=[O:13])[NH:8][C:7](=[O:15])[N:6]([NH:16][S:17]([CH3:20])(=[O:19])=[O:18])[C:5]2=[O:21].CO[CH:24]1[CH2:28][CH2:27][CH:26](OC)O1>C(O)(=O)C.C(OCC)C>[N+:12]([C:11]1[CH:10]=[C:9]2[C:4]([C:5](=[O:21])[N:6]([NH:16][S:17]([CH3:20])(=[O:18])=[O:19])[C:7](=[O:15])[NH:8]2)=[CH:3][C:2]=1[N:1]1[CH:24]=[CH:28][CH:27]=[CH:26]1)([O-:14])=[O:13]

참가 물질

5

반응물 2

HCID 790982,5-DimethoxytetrahydrofuranHCID 11674068N-(6-Amino-7-nitro-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)-methanesulfonamide

생성물 1

HCID 11545096N-(7-Nitro-2,4-dioxo-6-pyrrol-1-yl-1,4-dihydro-2H-quinazolin-3-yl)-methanesulfonamide

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 3283Diethyl Ether용매

실험 절차

A solution of N-(6-amino-7-nitro-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)-methanesulfonamide (90 mg, 0.285 mmol) and 2,5-dimethoxytetrahydrofuran (0.038 ml, 0.291 mmol) in acetic acid (0.5 ml) is refluxed for 80 minutes. The resulting suspension is filtered and the residue washed with ethyl acetate. The filtrate is concentrated in vacuo to give a brown solid which is suspended in diethyl ether and filtered to give a brown-orange solid as the desired pure product, m.p. 243-250° C.

후처리

  1. filtrationThe resulting suspension is filtered
  2. washthe residue washed with ethyl acetate
  3. concentrationThe filtrate is concentrated in vacuo
  4. customto give a brown solid which
  5. filtrationfiltered
  6. customto give a brown-orange solid as the desired pure product, m.p. 243-250° C.

출처 및 근거

ORD 기록
ord-57ac8f659f1e43e39a946cea55f4d616
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299085B2

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