Hydrochloric Acid → (E)-7-(5-amino-2-methylstyryl)thieno[3,2-d]pyrimidine-4-amine

HRID 1464981노트

반응식

HRID 1464981 반응식
[CH3:1][C:2]1[CH:19]=[CH:18][C:17]([N+:20]([O-])=O)=[CH:16][C:3]=1/[CH:4]=[CH:5]/[C:6]1[C:10]2[N:11]=[CH:12][N:13]=[C:14]([NH2:15])[C:9]=2[S:8][CH:7]=1.O.O.Cl[Sn]Cl.Cl.[NH4+].[OH-].C([O-])([O-])=O.[Na+].[Na+]>C(OCC)(=O)C>[NH2:20][C:17]1[CH:18]=[CH:19][C:2]([CH3:1])=[C:3]([CH:16]=1)/[CH:4]=[CH:5]/[C:6]1[C:10]2[N:11]=[CH:12][N:13]=[C:14]([NH2:15])[C:9]=2[S:8][CH:7]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 14923Ammonium HydroxideHCID 61436Stannous chloride dihydrateHCID 53357563(E)-7-(2-methyl-5-nitrostyryl)thieno[3,2-d]pyrimidine-4-amine

생성물 1

HCID 67359028(E)-7-(5-amino-2-methylstyryl)thieno[3,2-d]pyrimidine-4-amine수율 95.9%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

(E)-7-(2-methyl-5-nitrostyryl)thieno[3,2-d]pyrimidine-4-amine (0.3 g, 0.96 mmol) was dissolved in ethyl acetate (5 mL) and then SnCl2.2H2O (1 g, 4.81 mmol) and conc. HCl (0.5 mL) were added thereto, and the reaction mixture was stirred at room temperature for 18 hours. After the reaction was completed NH4OH solution was added thereto to pH 5. Then, anhydrous Na2CO3 was added thereto to pH 7. The reaction mixture was filtered with Celite and washed with ethyl acetate several times. The filtrate was concentrated under reduced pressure to obtain the title compound (260 mg, 84% yield) without further purification.

후처리

  1. additionwas added
  2. filtrationThe reaction mixture was filtered with Celite
  3. washwashed with ethyl acetate several times
  4. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d9b2d6f13d55416b84eb8a8676e51ad6
출처 데이터셋
uspto-grants-2015_04
특허 번호
US08999973B2

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