Diisopropylethylamine → 6-(2,5-Difluorophenyl)-3,4-dihydro-3-methylene-5-nitro-2H-pyran

HRID 923369노트

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HRID 923369 반응식
C(N(CC)C(C)C)(C)C.[N+:10]([CH2:13][C:14]([C:16]1[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:17]=1[F:23])=[O:15])([O-:12])=[O:11].I[CH2:25][C:26]([CH2:28]I)=[CH2:27]>CN(C)C=O>[CH2:25]=[C:26]1[CH2:28][C:13]([N+:10]([O-:12])=[O:11])=[C:14]([C:16]2[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:17]=2[F:23])[O:15][CH2:27]1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 110450293-Iodo-2-(iodomethyl)prop-1-eneHCID 57371203HCID 57371203, 화합물

생성물 1

HCID 575192486-(2,5-Difluorophenyl)-3,4-dihydro-3-methylene-5-nitro-2H-pyran

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

N,N-diisopropylethylamine (184 mL) was added to a solution of 2-nitro-1-(2,5-difluorophenyl)ethanone (92.7 g, 461 mmol) in N,N-dimethylformamide (1000 mL) and 3-iodo-2-(iodomethyl)prop-1-ene (156 g, 507 mmol). The mixture was heated at 60° C. for 2 h, evaporated and purified by chromatography (silica gel, gradient 0-30% dichloromethane in hexane) to yield 3-methylene-5-nitro-6-(2,5-difluorophenyl)-3,4-dihydro-2H-pyran.

후처리

  1. customevaporated
  2. custompurified by chromatography (silica gel, gradient 0-30% dichloromethane in hexane)

출처 및 근거

ORD 기록
ord-1d019067ccbd417db4610b2cbf2487a0
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09278976B2

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