Potassium Iodide → 4-Bromo-4'-decyloxybiphenyl

HRID 651312

反応式

HRID 651312 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.Br[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].C(=O)([O-])[O-].[K+].[K+].[I-].[K+].C(C1C=CC(C2C=CC(OCCCCCCCCCC)=CC=2)=CC=1)#N>CC(=O)CC>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])=[CH:10][CH:9]=2)=[CH:6][CH:7]=1

参加物

7

反応物 5

HCID 4875Potassium IodideHCID 81731-BromodecaneHCID 11430Potassium CarbonateHCID 950934-Bromo-4'-hydroxybiphenylHCID 112405[1,1'-Biphenyl]-4-carbonitrile, 4'-(decyloxy)-

生成物 1

HCID 106680514-Bromo-4'-decyloxybiphenyl

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

Quantities: 4-bromo-4′-hydroxybiphenyl (67) (20.00 g, 0.08 mol), 1-bromodecane (22.12 g, 0.10 mol), anhydrous potassium carbonate (57.10 g, 0.413 mol), potassium iodide (trace), butanone (500 ml). The experimental procedure was as described for the preparation of compound 57. The cooled mixture of product and inorganic salts was filtered off and washed carefully with dilute hydrochloric acid to remove the potassium carbonate. The white product was then washed with water until acid-free and heated under reflux with a minimum volume of ethanol to remove traces of 1-bromodecane. The product was filtered off, washed with cold ethanol and dried in vacuo to yield colourless crystals.

後処理

  1. additionThe cooled mixture of product and inorganic salts
  2. filtrationwas filtered off
  3. washwashed carefully with dilute hydrochloric acid
  4. customto remove the potassium carbonate
  5. washThe white product was then washed with water until acid-free and
  6. temperatureheated
  7. temperatureunder reflux with a minimum volume of ethanol
  8. customto remove traces of 1-bromodecane
  9. filtrationThe product was filtered off
  10. washwashed with cold ethanol
  11. customdried in vacuo
  12. customto yield colourless crystals

出典と根拠

ORDレコード
ord-bba584ad74224236a3aa681dde7db484
出典データセット
uspto-grants-2001_08
特許番号
US06278028B1

関連ノート

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