3-Ethoxy-2-methyl-2-propenal → HCID 12056717, 화합물

HRID 1060522노트

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HRID 1060522 반응식
O.O.Cl.[F:4][C:5]([F:16])([F:15])[C:6]1[CH:14]=[CH:13][C:9]([C:10]([NH2:12])=[NH:11])=[CH:8][CH:7]=1.C(O[CH:20]=[C:21]([CH3:24])[CH:22]=O)C.C[O-].[Na+]>CO>[CH3:24][C:21]1[CH:20]=[N:11][C:10]([C:9]2[CH:13]=[CH:14][C:6]([C:5]([F:15])([F:16])[F:4])=[CH:7][CH:8]=2)=[N:12][CH:22]=1

참가 물질

5

반응물 3

HCID 5591983-Ethoxy-2-methyl-2-propenalHCID 10942334Sodium MethoxideHCID 446307714-(Trifluoromethyl)benzene-1-carboximidamide--hydrogen chloride--water (1/1/2)

생성물 1

HCID 12056717HCID 12056717, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
50 °C

실험 절차

A sample of 4-trifluoromethylbenzamidine hydrochloride dihydrate (Maybridge, 15.2 g, 58 mmol) was dissolved in 100 mL of methanol and 3-ethoxy-2-methylacrolein (Janssen, 7.8 g, 64 mmol) was added. Sodium methoxide (25% solution in methanol, 14.7 mL) was added and the mixture was heated at 50° C. for 3 h. The cooled reaction mixture was then dded to 500 ml of ice water and stirred for 30 minutes. The white solid was filtered, air dried, dissolved in 300 mL of dichloromethane and dried over magnesium sulfate. The solvent was removed under reduced pressure to yield, after trituration with hexanes, 12.5 g of the product as a white solid melting at 143-146° C. 1H NMR (CDCl3): δ2.37 (s, 3H), 7.73 (d, 2H), 8.53 (d, 2H), 8.66 (s, 2H).

후처리

  1. customThe cooled reaction mixture
  2. filtrationThe white solid was filtered
  3. customair dried
  4. dissolutiondissolved in 300 mL of dichloromethane
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was removed under reduced pressure
  7. customto yield

출처 및 근거

ORD 기록
ord-8107a03512de4b559c7e3dba5f308ee3
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525001B1

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