Sodium hydride → HCID 59823036, 화합물

HRID 1260428

반응식

HRID 1260428 반응식
[H-].[Na+].[F:3][C:4]1[CH:9]=[C:8]([I:10])[CH:7]=[CH:6][C:5]=1[NH:11][C:12]1[C:21]2[C:20](=[O:22])[NH:19][CH:18]=[N:17][C:16]=2[N:15]([CH3:23])[C:14](=[O:24])[C:13]=1C.Cl[CH2:27][C@H:28]1[CH2:32][O:31][C:30]([CH3:34])([CH3:33])[O:29]1>CN(C=O)C>[CH3:33][C:30]1([CH3:34])[O:29][C@@H:28]([CH2:27][N:19]2[C:20](=[O:22])[C:21]3[C:12]([NH:11][C:5]4[CH:6]=[CH:7][C:8]([I:10])=[CH:9][C:4]=4[F:3])=[CH:13][C:14](=[O:24])[N:15]([CH3:23])[C:16]=3[N:17]=[CH:18]2)[CH2:32][O:31]1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 2734443(R)-(+)-4-(Chloromethyl)-2,2-dimethyl-1,3-dioxolaneHCID 1359290085-(2-Fluoro-4-iodophenylamino)-6,8-dimethylpyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione

생성물 1

HCID 59823036HCID 59823036, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

Sodium hydride (89 mg, 4.7 mmol, 5 eq) was stirred in anhydrous DMF (1 mL) for 10 minutes. 5-(2-Fluoro-4-iodophenylamino)-6,8-dimethylpyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione (400 mg, 0.94 mmol, 1 eq) in anhydrous DMF (400 μL) was added and the mixture stirred for 10 minutes. (R)-4-(Chloromethyl)-2,2-dimethyl-1,3-dioxolane (260 μl, 1.88 mmol, 2 eq) was added and the mixture subjected to microwave irradiation at 150° C. for 35 minutes. The solvent was removed in vacuo and the residue purified by HPLC. 1H NMR (400 MHz, MeOD) δ ppm 1.37 (s, 3H) 1.47 (s, 3H) 3.70 (s, 3H) 3.85 (dd, J=8.97, 5.68 Hz, 1H) 4.13 (dd, J=13.89, 7.07 Hz, 1H) 4.20 (dd, J=8.72, 6.69 Hz, 1H) 4.38 (dd, J=13.89, 3.03 Hz, 1H) 4.50-4.59 (m, 1H) 5.81 (s, 1H) 7.36 (t, J=8.21 Hz, 1H) 7.62-7.74 (m, 2H) 8.49 (s, 1H). [M+H] calc'd for C20H20FIN4O4, 527. found, 527.

후처리

  1. customirradiation at 150° C. for 35 minutes
  2. customThe solvent was removed in vacuo
  3. customthe residue purified by HPLC

출처 및 근거

ORD 기록
ord-4b714bd59d1740a297477035250a732d
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08470837B2

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