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Potassium Phosphate, Tribasic → 2-Fluoro-4-(4-methoxy-2-trifluoromethyl-phenylamino)-benzonitrile

HRID 1428202
ノート
印刷プレビュー

反応式

HRID 1428202 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]([F:13])([F:12])[F:11].[O-]P([O-])([O-])=O.[K+].[K+].[K+].CC(C1C=C(C(C)C)C(C2C=CC=CC=2P(C2CCCCC2)C2CCCCC2)=C(C(C)C)C=1)C.Br[C:57]1[CH:64]=[CH:63][C:60]([C:61]#[N:62])=[C:59]([F:65])[CH:58]=1>C1(C)C=CC=CC=1>[F:65][C:59]1[CH:58]=[C:57]([NH:1][C:2]2[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=2[C:10]([F:11])([F:12])[F:13])[CH:64]=[CH:63][C:60]=1[C:61]#[N:62]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 7360294-Bromo-2-fluorobenzonitrileHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenylHCID 226017214-Methoxy-2-(trifluoromethyl)aniline

生成物 1

HCID 667656782-Fluoro-4-(4-methoxy-2-trifluoromethyl-phenylamino)-benzonitrile収率 87%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
110 °C

実験手順

2-Amino-5-methoxy-benzotrifluoride (10.46 mmol), K3PO4 (15.7 mmol), Xphos (1.05 mmol) and Pd4(dba)3 (0.314 mmol) were added under nitrogen to a solution of 4-bromo-2-fluoro-benzonitrile (10.46 mmol) in 50 mL toluene and the mixture was stirred for 20 hours at a bath temperature of 110° C. Then the mixture was filtered through a glass fibre filter, then the filtrate was extracted with 150 mL water. The organic phase was dried on sodium sulphate and evaporated down. In this way the product was obtained in a yield of 87% of theory.

後処理

  1. filtrationThen the mixture was filtered through a glass fibre
  2. filtrationfilter
  3. extractionthe filtrate was extracted with 150 mL water
  4. customThe organic phase was dried on sodium sulphate
  5. customevaporated down
  6. customIn this way the product was obtained in a yield of 87% of theory

出典と根拠

ORDレコード
ord-16fef055e3bb4594b4fe0f5f07f37451
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08937073B2

反応ノート

読み込み中…

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