Stannous chloride dihydrate → HCID 18516946, 화합물

HRID 1370093노트

반응식

HRID 1370093 반응식
[C:1]([C:3]1[C:4]([C:19]2[S:20][CH:21]=[CH:22][CH:23]=2)=[N:5][C:6]([NH:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([N+:16]([O-])=O)[CH:11]=2)=[N:7][CH:8]=1)#[N:2].O.O.[Sn](Cl)Cl>C(O)C>[NH2:16][C:12]1[CH:11]=[C:10]([NH:9][C:6]2[N:5]=[C:4]([C:19]3[S:20][CH:21]=[CH:22][CH:23]=3)[C:3]([C:1]#[N:2])=[CH:8][N:7]=2)[CH:15]=[CH:14][CH:13]=1

참가 물질

4

반응물 2

HCID 61436Stannous chloride dihydrateHCID 18516888HCID 18516888, 화합물

생성물 1

HCID 18516946HCID 18516946, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

N-3-Aminophenyl-5-cyano-4-thien-2-ylpyrimidine-2-amine was prepared by heating a solution of 5-cyano-N-3-nitrophenyl-4-thien-2-ylpyrimidine-2-amine (2.77 g, 8.57 mmol) and tin(II)chloride dihydrate (7.73 g, 34.05 mmol) in ethanol (160 mL) at reflux for 18 h. On cooling the reaction was concentrated under reduced pressure and partitioned between CH2Cl2 and 2M NaOH. The organic phase was dried (MgSO4) and evaporated to give the desired material (320 mg) as a yellow solid, m.p. 221-222°. δH (d6 DMSO) 10.16 (1H, s), 8.83 (1H, s), 8.24 (1H, d, J 3.9 Hz), 7.97 (1H, d, J 5.1 Hz), 7.32 (1H, dd, J 5.0, 4.0 Hz), 6.97 (3H, bm), 6.31 (1H, m) and 5.04 (2H, bs).

후처리

  1. temperatureat reflux for 18 h
  2. temperatureOn cooling the reaction
  3. concentrationwas concentrated under reduced pressure
  4. custompartitioned between CH2Cl2 and 2M NaOH
  5. dry with materialThe organic phase was dried (MgSO4)
  6. customevaporated

출처 및 근거

ORD 기록
ord-f4a2f86685fa459a8ba83ed881e0b6f1
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06579983B1

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