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Cesium carbonate → methyl 4-(chroman-6-yl)-6-methyl-1H-pyrrolo[2,3-b]pyridine-5-carboxylate

HRID 1912545
ノート
印刷プレビュー

反応式

HRID 1912545 の反応式
[NH2:1][C:2]1[C:11]([CH:12]=O)=[C:10]([C:14]2[CH:15]=[C:16]3[C:21](=[CH:22][CH:23]=2)[O:20][CH2:19][CH2:18][CH2:17]3)[C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([CH3:24])[N:3]=1.[C:25](=O)([O-])[O-].[Cs+].[Cs+].[Si](C=[N+]=[N-])(C)(C)C>CO>[O:20]1[C:21]2[C:16](=[CH:15][C:14]([C:10]3[C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([CH3:24])[N:3]=[C:2]4[NH:1][CH:25]=[CH:12][C:11]=34)=[CH:23][CH:22]=2)[CH2:17][CH2:18][CH2:19]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 10796Cesium carbonateHCID 167693TrimethylsilyldiazomethaneHCID 86675740Methyl 6-amino-4-(chroman-6-yl)-5-formyl-2-methylnicotinate

生成物 1

HCID 71209166methyl 4-(chroman-6-yl)-6-methyl-1H-pyrrolo[2,3-b]pyridine-5-carboxylate収率 97%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
55 °C

実験手順

A mixture of methyl 6-amino-4-(chroman-6-yl)-5-formyl-2-methylnicotinate (4.5 g, 13.79 mmol) and cesium carbonate (8.99 g, 27.6 mmol) in methanol (180 mL) was heated to 55° C. and then treated with TMSCHN2, 2.0 M solution in hexanes (27.6 mL, 55.2 mmol). The mixture was heated to 60° C. for several minutes until LCMS and TLC showed the reaction was complete. The mixture was cooled in an ice-bath and then quenched with saturated ammonium chloride. The mixture was extracted with ethyl acetate. The extracts were washed with brine, dried over sodium sulfate, filtered and concentrated to afford the crude product (4.3 g, 13.34 mmol, 97% yield) as a pale yellow solid: 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 7.34 (br. s., 1 H), 7.28-7.21 (m, 2 H), 6.93-6.87 (m, 1 H), 6.48 (d, J=2.9 Hz, 1 H), 4.30-4.25 (m, 2 H), 3.72-3.68 (m, 3 H), 2.90-2.83 (m, 2 H), 2.74 (s, 3 H), 2.12-2.05 (m, 2 H); LC/MS (m/z) ES+=323.24 (M+1).

後処理

  1. temperatureThe mixture was heated to 60° C. for several minutes until LCMS and TLC
  2. temperatureThe mixture was cooled in an ice-bath
  3. customquenched with saturated ammonium chloride
  4. extractionThe mixture was extracted with ethyl acetate
  5. washThe extracts were washed with brine
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-f0dc20f497ba4faaa1258943a3315b6a
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08609653B2

反応ノート

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