Diethyl Ether → 6-Nitro-9-(thiophene-2-sulfonyl)-1,4,7,8,9,10-hexahydro-pyrido[3,4-f]quinoxaline-2,3-dione

HRID 1739676ノート

反応式

HRID 1739676 の反応式
[N+:1]([C:4]1[C:13]2[N:14]=[CH:15][CH:16]=[CH:17][C:12]=2[C:11]2[C:6](=[N:7][C:8](=[O:19])[C:9](=[O:18])[N:10]=2)[CH:5]=1)([O-:3])=[O:2].Cl[S:21]([C:24]1[S:25][CH:26]=[CH:27][CH:28]=1)(=[O:23])=[O:22].C(N(CC)CC)C.C(OCC)C>C1COCC1.CN(C=O)C>[N+:1]([C:4]1[C:17]2[CH2:16][CH2:15][N:14]([S:21]([C:24]3[S:25][CH:26]=[CH:27][CH:28]=3)(=[O:23])=[O:22])[CH2:13][C:12]=2[C:11]2[NH:10][C:9](=[O:18])[C:8](=[O:19])[NH:7][C:6]=2[CH:5]=1)([O-:3])=[O:2]

参加物

7

反応物 4

HCID 3283Diethyl EtherHCID 8471TriethylamineHCID 855182-Thiophenesulfonyl chlorideHCID 727442526-Nitropyridoquinoxalinedione

生成物 1

HCID 218369506-Nitro-9-(thiophene-2-sulfonyl)-1,4,7,8,9,10-hexahydro-pyrido[3,4-f]quinoxaline-2,3-dione収率 52%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

A mixture of the 6-nitropyridoquinoxalinedione (0.1 g, 0.38 mmol), 2-chlorosulfonyl thiophene (104 mg, 0.57 mmol), triethylamine (70 μl) in THF (5 mL) and DMF (5 mL) was stirred at 60° C. for 24 hours. The mixture was poured onto water and diethyl ether. The precipitate was collected by filtration, washed with water and ether, and dried in vacuo to give product as a yellow solid (80 mg) in 52% yield; mp >300° C. m/e, M+1 409 nmR, IR, CHN.

後処理

  1. filtrationThe precipitate was collected by filtration
  2. washwashed with water and ether
  3. customdried in vacuo

出典と根拠

ORDレコード
ord-f8d22c6dac5d41ce86ba8e324e8b06f6
出典データセット
uspto-grants-1999_10
特許番号
US05968928

反応ノート

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