Water → HCID 46182258、化合物

HRID 450582ノート

反応式

HRID 450582 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 46182258HCID 46182258、化合物収率 63.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-f65ee6a7b4204ab6971f068f7683a86d
出典データセット
uspto-grants-2013_07
特許番号
US08486953B2

反応ノート

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