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

HRID 1098328ノート

反応式

HRID 1098328 の反応式
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

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 110450293-Iodo-2-(iodomethyl)prop-1-eneHCID 57371203HCID 57371203、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-e6af30de57ee44e58c505a12a2285efc
出典データセット
uspto-grants-2012_03
特許番号
US08143289B2

反応ノート

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