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

HRID 2069198ノート

反応式

HRID 2069198 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-57ac8f659f1e43e39a946cea55f4d616
出典データセット
uspto-grants-2012_10
特許番号
US08299085B2

反応ノート

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