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

HRID 1739676노트

반응식

HRID 1739676 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f8d22c6dac5d41ce86ba8e324e8b06f6
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05968928

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