Toluene → HCID 178435532、化合物

HRID 1368558ノート

反応式

HRID 1368558 の反応式
BrC1C=C2C(=CC=1)[CH:8]=[C:7]([C:12]([C:17]1[N:18]=[CH:19][N:20](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH:21]=1)([OH:16])[CH:13]([CH3:15])[CH3:14])[CH:6]=[CH:5]2.[CH2:41](C([Sn])=C(CCCC)CCCC)CCC.[C:56]1([CH3:62])[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=1>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:62]([C:56]1[CH:61]=[C:60]2[C:59](=[CH:58][CH:57]=1)[CH:8]=[C:7]([C:12]([C:17]1[N:18]=[CH:19][NH:20][CH:21]=1)([OH:16])[CH:13]([CH3:15])[CH3:14])[CH:6]=[CH:5]2)[CH3:41]

参加物

5

反応物 3

HCID 1140TolueneHCID 22018349HCID 22018349、化合物HCID 53438229Tri(butyl)vinyltin

生成物 1

HCID 178435532HCID 178435532、化合物

試薬・触媒・溶媒 1

HCID 178418397HCID 178418397、化合物触媒

実験手順

A solution of 1-(6-bromonaphthalen-2-yl)-2-methyl-1-(1-trityl-1H-imidazol-4-yl)-1-propanol (2.0 g), tetrakis(triphenylphosphine)palladium (116 mg) and tributylvinyltin (1.40 ml) in toluene (30 ml) was refluxed under argon atmosphere for 80 min. The solvent was distilled off and the residue was purified by column chromatography (eluent, hexane:THF=2:1),then crystallized from isopropyl ether-hexane (1:1) to give the titled compound (1.47 g) as a colorless powder.

後処理

  1. distillationThe solvent was distilled off
  2. customthe residue was purified by column chromatography (eluent, hexane
  3. customTHF=2:1),then crystallized from isopropyl ether-hexane (1:1)

出典と根拠

ORDレコード
ord-9f165b7ede0e476da5876cebb700d18a
出典データセット
uspto-grants-2003_06
特許番号
US06573289B1

反応ノート

読み込み中…