Water → HCID 46182258, 화합물

HRID 450582

반응식

HRID 450582 반응식
C[C:2]1[N:3]=[C:4]([NH:15][C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][C:17]=2[O:23][CH:24]2[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]2)[C:5]2[C:10]([CH3:11])=[C:9]([C:12]([NH2:14])=[O:13])[S:8][C:6]=2[N:7]=1.CCN(C(C)C)C(C)C.Cl[CH2:40][C:41]1[N:45]=[CH:44][O:43][N:42]=1.O>CN(C=O)C>[O:43]1[CH:44]=[N:45][C:41]([CH2:40][N:27]2[CH2:28][CH2:29][CH:24]([O:23][C:17]3[CH:18]=[C:19]([F:22])[CH:20]=[CH:21][C:16]=3[NH:15][C:4]3[C:5]4[C:10]([CH3:11])=[C:9]([C:12]([NH2:14])=[O:13])[S:8][C:6]=4[N:7]=[CH:2][N:3]=3)[CH2:25][CH2:26]2)=[N:42]1

참가 물질

6

반응물 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 27357653-(Chloromethyl)-1,2,4-oxadiazoleHCID 69669337HCID 69669337, 화합물

생성물 1

HCID 46182258HCID 46182258, 화합물수율 63.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

To a suspension of methyl 4-(4-fluoro-2-(piperidin-4-yloxy)phenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxamide (0.06 g, 0.15 mmol) in DMF (2.0 mL) was added Hünigs base (0.06 mL, 0.35 mmol) and 3-(chloromethyl)-1,2,4-oxadiazole (0.035 g, 0.3 mmol) and the mixture was warmed to 60° C. for 18 hours. After cooling to ambient temperature water (2 mL) was added and the mixture stirred for 0.5 hours. The precipitated solid was collected by filtration and triturated from boiling MeCN. The solid was collected by filtration and dried under vacuum to give beige solid (0.046 g, 63%).

후처리

  1. additionwas added
  2. filtrationThe precipitated solid was collected by filtration
  3. customtriturated
  4. filtrationThe solid was collected by filtration
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-f65ee6a7b4204ab6971f068f7683a86d
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486953B2

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