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Sodium Carbonate → HCID 178419853、化合物

HRID 1846805
ノート
印刷プレビュー

反応式

HRID 1846805 の反応式
[O:1]1[CH2:6][CH:5]=[C:4](B2OC(C)(C)C(C)(C)O2)[CH2:3][CH2:2]1.Cl[C:17]1[C:18]([O:23][C@H:24]2[CH2:29][CH2:28][C@H:27]([NH:30][C:31]3[S:32][C:33]4[CH:39]=[CH:38][CH:37]=[CH:36][C:34]=4[N:35]=3)[CH2:26][CH2:25]2)=[N:19][CH:20]=[CH:21][N:22]=1.C(=O)([O-])[O-].[Na+].[Na+]>COCCOC>[O:1]1[CH2:6][CH:5]=[C:4]([C:17]2[C:18]([O:23][C@H:24]3[CH2:25][CH2:26][C@H:27]([NH:30][C:31]4[S:32][C:33]5[CH:39]=[CH:38][CH:37]=[CH:36][C:34]=5[N:35]=4)[CH2:28][CH2:29]3)=[N:19][CH:20]=[CH:21][N:22]=2)[CH2:3][CH2:2]1
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

5

反応物 3

HCID 10340Sodium CarbonateHCID 112180533,6-Dihydro-2H-pyran-4-boronic acid pinacol esterHCID 178478365HCID 178478365、化合物

生成物 1

HCID 178419853HCID 178419853、化合物収率 83%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
80 °C

実験手順

A mixture of 2-(3,6-dihydro-2H-pyran-4-yl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (0.10 g, 0.49 mmol) and N-(trans-4-(3-chloropyrazin-2-yloxy)cyclohexyl)benzo[d]thiazol-2-amine (0.14 g, 0.39 mmol), prepared as in step 1 of example 9a, in 1,2-dimethoxyethane (2 mL) and aqueous sodium carbonate (2 M, 0.58 mL, 1.16 mmol) was placed under nitrogen atmosphere using 3 evacuation/backfill cycles. Tetrakis triphenylphosphine(palladium) (0.022 g, 0.019 mmol) was added and one more evacuation/backfill cycle was executed. The mixture was then heated to 80° C. After 4 h the mixture was cooled to RT and partitioned between ethyl acetate and water. The layers were separated and the aqueous layer was extracted with ethyl acetate twice. The combined extracts were dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. The resulting oil was purified by silica gel chromatography to give N-(trans-4-(3-(3,6-dihydro-2H-pyran-4-yl)pyrazin-2-yloxy)cyclohexyl)benzo[d]thiazol-2-amine (0.13 g, 0.32 mmol, 83% yield). [M+1] 409.2. IC50 (uM): 0.03702.

後処理

  1. temperatureAfter 4 h the mixture was cooled to RT
  2. custompartitioned between ethyl acetate and water
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with ethyl acetate twice
  5. dry with materialThe combined extracts were dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe resulting oil was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-e1a05b964c6b4c74bd1da79aadef8269
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952037B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート