Hydrazine → 4-Hydrazino-2-(trifluoromethyl)quinazoline

HRID 2063590

反応式

HRID 2063590 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([C:12]([F:15])([F:14])[F:13])[N:3]=1.[NH2:16][NH2:17].C(=O)([O-])[O-].[K+].[K+]>O1CCCC1>[F:13][C:12]([F:15])([F:14])[C:4]1[N:3]=[C:2]([NH:16][NH2:17])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=1

参加物

5

反応物 3

HCID 9321HydrazineHCID 11430Potassium CarbonateHCID 14754354-chloro-2-(trifluoromethyl)quinazoline

生成物 1

HCID 14754644-Hydrazino-2-(trifluoromethyl)quinazoline収率 56.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 4-chloro-2-(trifluoromethyl)quinazoline (2.0 g, 8.6 mmol) and hydrazine (0.27 mL, 8.6 mmol) in 20 mL of tetrahydrofuran was added 1.8 g (13 mmol) of potassium carbonate. The resultant suspension was stirred at ambient temperature for 2 hours. The reaction mixture was partitioned between ethyl acetate and water. The aqueous layer was extracted with ethyl acetate and the combined organics were dried over magnesium sulfate. After filtration, the organics were concentrated in vacuo to yield a yellow solid that was recrystallized in ethyl acetate:hexanes. 1.1 g (56%) of yellow needle-like crystals were isolated.

後処理

  1. customThe reaction mixture was partitioned between ethyl acetate and water
  2. extractionThe aqueous layer was extracted with ethyl acetate
  3. dry with materialthe combined organics were dried over magnesium sulfate
  4. filtrationAfter filtration
  5. concentrationthe organics were concentrated in vacuo
  6. customto yield a yellow solid
  7. customthat was recrystallized in ethyl acetate

出典と根拠

ORDレコード
ord-393a81e8894d48a09d519c362141752b
出典データセット
uspto-grants-2012_10
特許番号
US08288398B2

関連ノート

読み込み中…