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1,2,4-Trimethylbenzene → HCID 86701346、化合物

HRID 2179847
ノート
印刷プレビュー

反応式

HRID 2179847 の反応式
[C:1]1([C:11]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[C:18](B(O)O)=[C:17]3[C:12]=2[CH:13]=[CH:14][CH:15]=[CH:16]3)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.FC(F)(F)S(O[C:34]1[CH:43]=[CH:42][C:41]2[C:36](=[CH:37][C:38]([O:44][CH3:45])=[CH:39][CH:40]=2)[CH:35]=1)(=O)=O.P([O-])([O-])([O-])=O.[K+].[K+].[K+].C1(C(=CC(=CC=1)C)C)C>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.O.CC(O)C>[CH3:45][O:44][C:38]1[CH:37]=[C:36]2[C:41]([CH:42]=[CH:43][C:34]([C:18]3[C:17]4[C:12]([C:11]([C:1]5[C:10]6[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=6)[CH:4]=[CH:3][CH:2]=5)=[C:24]5[C:19]=3[CH:20]=[CH:21][CH:22]=[CH:23]5)=[CH:13][CH:14]=[CH:15][CH:16]=4)=[CH:35]2)=[CH:40][CH:39]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 72471,2,4-TrimethylbenzeneHCID 62657Potassium Phosphate, TribasicHCID 10892112Methanesulfonic acid, trifluoro-, 7-methoxy-2-naphthalenyl esterHCID 23088558[10-(Naphthalen-1-yl)anthracen-9-yl]boronic acid

生成物 1

HCID 86701346HCID 86701346、化合物収率 52.7%

試薬・触媒・溶媒 3

HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒2 回
HCID 3776Isopropanol溶媒

実験手順

Under the nitrogen atmosphere, (10-(naphthalen-1-yl)anthracen-9-yl)boronic acid (25.1 g), 7-methoxynaphthalen-2-yl trifluoromethane sulfonate (24.3 g), Pd(PPh3)4 (0.9 g), potassium phosphate (30.6 g), and a mixture solvent (260 ml) of pseudo cumene, IPA, and water (pseudo cumene/IPA/water=8/4/1 (volume ratio)) were added to a flask and refluxed for 4.5 hours. Once the heating is completed, water was added. After cooling to room temperature, a solid was collected by suction filtration. The obtained solid was washed with water and subsequently with methanol, dissolved in toluene, and purified with a silica gel short column. Crystals obtained by slow distillation of the solvent under reduced pressure were collected by suction filtration to give 9-(7-methoxynaphthalen-2-yl)-10-(naphthalen-1-yl)anthracene (17.5 g) as a third intermediate compound. The scheme is shown in the following “Reaction 4”.

後処理

  1. temperaturerefluxed for 4.5 hours
  2. filtrationa solid was collected by suction filtration
  3. washThe obtained solid was washed with water and subsequently with methanol
  4. dissolutiondissolved in toluene
  5. custompurified with a silica gel short column
  6. customCrystals obtained by slow distillation of the solvent under reduced pressure
  7. filtrationwere collected by suction filtration

出典と根拠

ORDレコード
ord-046678364a4646ae9a449b0b6bb6b3d4
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09070885B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート