Sodium Carbonate → 9-(Naphthalen-2-yl)anthracene

HRID 1506274ノート

反応式

HRID 1506274 の反応式
Br[C:2]1[C:3]2[C:8]([CH:9]=[C:10]3[C:15]=1[CH:14]=[CH:13][CH:12]=[CH:11]3)=[CH:7][CH:6]=[CH:5][CH:4]=2.B(O)O.C(=O)([O-])[O-].[Na+].[Na+]>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.C1(C)C=CC=CC=1>[CH:4]1[C:3]2[C:2](=[CH:15][CH:10]=[CH:9][CH:8]=2)[CH:6]=[CH:5][C:4]=1[C:3]1[C:2]2[C:11]([CH:10]=[C:9]3[C:8]=1[CH:7]=[CH:7][CH:6]=[CH:5]3)=[CH:12][CH:13]=[CH:14][CH:15]=2

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 61668Boronic AcidHCID 740629-Bromoanthracene

生成物 1

HCID 2644169-(Naphthalen-2-yl)anthracene収率 173.5%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 1140Toluene溶媒

実験手順

22.5 g of 9-bromoanthracene, 15.8 g of 2-naphthelene boronic acid and 2.0 g of tetrakis(triphenylphosphine)palladium were mixed, followed by argon displacement. After adding 150 ml of toluene and 140 ml of 2M sodiumcarbonate aqueous solution thereto, it was refluxed on heating for 7 hours. After standing to cool, the crystal precipitated was filtrated it was washed by ethanol and toluene. The crystal obtained was recrystallized in toluene, followed by filtering and drying, and then 23.1 g of 9-(naphthalene-2-yl)anthracene was obtained (yield: 87%).

後処理

  1. temperatureit was refluxed
  2. temperatureon heating for 7 hours
  3. temperatureto cool
  4. customthe crystal precipitated
  5. filtrationwas filtrated it
  6. washwas washed by ethanol and toluene
  7. customThe crystal obtained
  8. customwas recrystallized in toluene
  9. filtrationby filtering
  10. customdrying

出典と根拠

ORDレコード
ord-37c041a24d2a49a78bc8fc470921c6ee
出典データセット
uspto-grants-2015_12
特許番号
US09219234B2

反応ノート

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