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

HRID 2280365

반응식

HRID 2280365 반응식
[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

참가 물질

8

반응물 4

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

생성물 2

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

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 887Methanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-a4026af5f96145e1a1263c9b7eb65129
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09139522B2

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