Bromine → HCID 20231438, 화합물

HRID 2290557노트

반응식

HRID 2290557 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:4]=1[C:12]1[S:13][CH:14]=[CH:15][CH:16]=1.[Br:17]Br.S([O-])([O-])=O.[Na+].[Na+]>C(OCC)C.O1CCOCC1>[Br:17][C:14]1[S:13][C:12]([C:4]2[CH:5]=[CH:6][C:7]([N+:9]([O-:11])=[O:10])=[CH:8][C:3]=2[O:2][CH3:1])=[CH:16][CH:15]=1

참가 물질

6

반응물 3

HCID 24408BromineHCID 24437Sodium SulfiteHCID 13768627Thiophene, 2-(2-methoxy-4-nitrophenyl)-

생성물 1

HCID 20231438HCID 20231438, 화합물수율 90.8%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 312751,4-Dioxane용매

실험 절차

To a stirred 0° C. mixture of 8.0 g (0.034 mole) of 2-(2-methoxy-4-nitrophenyl)thiophene (Example 4, Step A) in 180 ml of diethyl ether was added a mixture of 10.8 g (0.07 mole) of bromine in 15.0 ml of 1,4-dioxane and 20 ml of diethyl ether. The mixture was allowed to warm to room temperature and stir for approximately 18 hours. The reaction mixture was poured into a mixture of sodium sulfite and ice water. The resultant mixture was extracted with diethyl ether, and the extract dried over anhydrous sodium sulfate. The dried extract was filtered, and the solvent evaporated from the filtrate to leave a residue. The residue was purified by column chromatography using silica gel and eluting with toluene to yield 9.7 g of 2-bromo-5-(2-methoxy-4-nitrophenyl)thiophene.

후처리

  1. additionwas added
  2. extractionThe resultant mixture was extracted with diethyl ether
  3. dry with materialthe extract dried over anhydrous sodium sulfate
  4. extractionThe dried extract
  5. filtrationwas filtered
  6. customthe solvent evaporated from the filtrate
  7. customto leave a residue
  8. customThe residue was purified by column chromatography
  9. washeluting with toluene

출처 및 근거

ORD 기록
ord-9c71a027f3f544d6a3cfe3aa4da726ad
출처 데이터셋
uspto-grants-1986_10
특허 번호
US04617316

반응 노트

불러오는 중…