Iodine → 1~4~-Iodo-1~1~,2~1~:2~3~,3~1~-terphenyl

HRID 2280365

反応式

HRID 2280365 の反応式
[C:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.O.[IH:21].II.S(=O)(=O)(O)O>CO.C(O)(=O)C>[C:1]1([C:7]2[CH:8]=[C:9]([C:13]3[CH:14]=[CH:15][C:16]([I:21])=[CH:17][CH:18]=3)[CH:10]=[CH:11][CH:12]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1.[C:1]1([C:7]2[CH:8]=[C:9]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH:10]=[C:11]([I:21])[CH:12]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

8

反応物 4

HCID 807IodineHCID 1118Sulfuric AcidHCID 7076M-TerphenylHCID 85613701Hydroiodic acid dihydrate

生成物 2

HCID 123784021~4~-Iodo-1~1~,2~1~:2~3~,3~1~-terphenylHCID 130672305'-Iodo-m-terphenyl

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 887Methanol溶媒

実験手順

A three-necked flask was charged with 250 g of m-terphenyl (ALDRICH), 50 g of hydroiodic acid dihydrate, 75 g of iodine, 750 ml of acetic acid, and 25 ml of concentrated sulfuric acid, and reaction was allowed to proceed at 70° C. for 3 hours. The product was poured into 5 L of methanol and the mixture was stirred for 1 hour and filtrated. The obtained crystals were purified by column chromatography, and recrystallized from acetonitrile to give 64 g of 3′-phenyl-4-iodobiphenyl (Intermediate 4) and 17 g of 3-phenyl-5-iodobiphenyl in the form of white powder. FD-MS and H-NMR analysis identified the powder as Intermediate 4.

後処理

  1. filtrationfiltrated
  2. customThe obtained crystals were purified by column chromatography
  3. customrecrystallized from acetonitrile

出典と根拠

ORDレコード
ord-a4026af5f96145e1a1263c9b7eb65129
出典データセット
uspto-grants-2015_09
特許番号
US09139522B2

関連ノート

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