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Ethyl Acetate → HCID 131735113、化合物

HRID 929251
ノート
印刷プレビュー

反応式

HRID 929251 の反応式
C([N:4]1[C:12]2[C:7](=[N:8][C:9](I)=[C:10]([Cl:13])[CH:11]=2)[N:6]=[C:5]1[O:15][C@@H:16]1[CH2:20][O:19][C@@H:18]2[C@H:21]([O:24][Si:25]([C:28]([CH3:31])([CH3:30])[CH3:29])([CH3:27])[CH3:26])[CH2:22][O:23][C@H:17]12)C=C.[CH:32]1([C:35]2[C:40]3[N:41]=[CH:42][S:43][C:39]=3[CH:38]=[CH:37][N:36]=2)[CH2:34][CH2:33]1.C(=O)([O-])[O-].[Cs+].[Cs+].CCOC(C)=O>CN(C=O)C.[Cu]I>[Si:25]([O:24][C@H:21]1[CH:18]2[O:19][CH2:20][C@@H:16]([O:15][C:5]3[NH:4][C:12]4[C:7]([N:6]=3)=[N:8][C:9]([C:42]3[S:43][C:39]5[CH:38]=[CH:37][N:36]=[C:35]([CH:32]6[CH2:33][CH2:34]6)[C:40]=5[N:41]=3)=[C:10]([Cl:13])[CH:11]=4)[CH:17]2[O:23][CH2:22]1)([C:28]([CH3:30])([CH3:29])[CH3:31])([CH3:26])[CH3:27]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8857Ethyl AcetateHCID 10796Cesium carbonateHCID 585705244-Cyclopropyl[1,3]thiazolo[4,5-c]pyridineHCID 123197088HCID 123197088、化合物2 回

生成物 1

HCID 131735113HCID 131735113、化合物

試薬・触媒・溶媒 2

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

Palladium tetrakistriphenylphosphine (200.0 mg, 0.173 mmol) was added to a stirred suspension of [(3R,3aR,6R,6aS)-3-(1-allyl-6-chloro-5-iodo-imidazo[4,5-b]pyridin-2-yl)oxy-2,3,3a,5,6,6a-hexahydrofuro[3,2-b]furan-6-yl]oxy-tert-butyl-dimethyl-silane (500.0 mg, 0.865 mmol, Intermediate 5), 4-cyclopropylthiazolo[4,5-c]pyridine (183.0 mg, 1.038 mmol), cesium carbonate (1.409 g, 4.33 mmol), and copper (I) iodide (99.0 mg, 0.519 mmol) in degassed DMF (3.2 mL). The reaction mixture placed under nitrogen before being heated to 100° C. for 3 h. The reaction mixture was cooled to room temperature and added to EtOAc (80 ml). The mixture filtered and the solids washed with EtOAc (2×30 mL). The filtrate was evaporated under reduced pressure. Flash chromatography of the resulting residue utilizing a 40 g silica RediSep Rf® Gold column and employing a 0-100% EtOAc/hexane gradient afforded the title compound. LC-MS: calculated for C27H32ClN5O4SSi 585.16 observed m/e: 586.17 (M+H)+ (Rt 1.18/1.8 min)

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationThe mixture filtered
  3. washthe solids washed with EtOAc (2×30 mL)
  4. customThe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-4a8932f3c3174ef2bef90f831f6e56d6
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09290517B2

反応ノート

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