Iodine → 5'-Iodo-m-terphenyl

HRID 470917

反応式

HRID 470917 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:12]=[C:11]([I:21])[CH:10]=[C:9]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

7

反応物 4

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

生成物 1

HCID 130672305'-Iodo-m-terphenyl収率 58.9%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 887Methanol溶媒

実験手順

A three neck flask was charged with 250 g of m-terphenyl (manufactured by Aldrich Co., Ltd.), 50 g of hydroiodic acid dihydrate, 75 g of iodine, 750 mL of acetic acid and 25 mL of cone, sulfuric acid, and they were reacted at 70° C. for 3 hours. After reaction, the solution was poured into 5 L of methanol and then stirred for one hour. This was separated by filtration, and crystal obtained was refined by means of column chromatography and recrystallized from acetonitrile to obtain 64 g of 5-phenyl-3-iodobiphenyl (intermediate 3) shown, below and 17 g of 3′-phenyl-4-iodobiphenyl (intermediate 4) shown below.

後処理

  1. customwere reacted at 70° C. for 3 hours
  2. customAfter reaction
  3. customThis was separated by filtration, and crystal
  4. customobtained
  5. customrecrystallized from acetonitrile

出典と根拠

ORDレコード
ord-1799225de70548219040d4c1b7dc07cf
出典データセット
uspto-grants-2014_01
特許番号
US08629613B2

関連ノート

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