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1-Butanol → ethyl 3-tosyl-3H-imidazo[1,2-a]pyrrolo[2,3-e]pyrazine-8-carboxylate

HRID 1969687
ノート
印刷プレビュー

反応式

HRID 1969687 の反応式
Cl[CH:2]([CH:8]=O)[C:3]([O:5][CH2:6][CH3:7])=[O:4].[S:10]([N:20]1[C:28]2[C:23](=[N:24][C:25]([NH2:29])=[CH:26][N:27]=2)[CH:22]=[CH:21]1)([C:13]1[CH:19]=[CH:18][C:16]([CH3:17])=[CH:15][CH:14]=1)(=[O:12])=[O:11].C(O)CCC>O1CCOCC1>[S:10]([N:20]1[C:28]2[N:27]=[CH:26][C:25]3[N:24]([C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])=[CH:8][N:29]=3)[C:23]=2[CH:22]=[CH:21]1)([C:13]1[CH:14]=[CH:15][C:16]([CH3:17])=[CH:18][CH:19]=1)(=[O:11])=[O:12]
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 2631-ButanolHCID 118030Ethyl (chloroformyl)acetate2 回HCID 580099825-tosyl-5H-pyrrolo[2,3-b]pyrazin-2-amine

生成物 1

HCID 58557515ethyl 3-tosyl-3H-imidazo[1,2-a]pyrrolo[2,3-e]pyrazine-8-carboxylate収率 60%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

反応条件

温度
80 °C

実験手順

A solution of ethyl 2-chloro-3-oxopropanoate (1.60 g, 7.65 mmol, prepared as described in US2009005359A1) and 1,4-dioxane (10.0 mL) was added to 5-tosyl-5H-pyrrolo[3,2-b]pyrazin-2-amine (1.45 g, 5.03 mmol, Preparation #E.1.1) under nitrogen. Anhydrous butan-1-ol (30.0 mL) was added, a reflux condenser was attached, and the system was sealed. After about 30 min, the mixture was warmed to about 80° C. The solution was allowed to cool to ambient temperature. A solution of ethyl 2-chloro-3-oxopropanoate (2.78 g, 13.3 mmol) and 1,4-dioxane (5 mL) was added. After about 30 min, the reaction mixture was warmed to about 80° C. After about 30 min, the mixture was warmed to about 125° C. After about 48 h, the brown solution was allowed to cool to ambient temperature. The volatiles were removed under reduced pressure. The residue was purified by silica gel chromatography eluting with a gradient of 5-50% EtOAc in heptane to give ethyl 3-tosyl-3H-imidazo[1,2-a]pyrrolo[2,3-e]pyrazine-8-carboxylate (1.16 g, 60%): LC/MS (Table 1, Method b) Rt=2.52 min; MS m/z 385 (M+H)+.

後処理

  1. customa reflux condenser was attached
  2. customthe system was sealed
  3. temperatureto cool to ambient temperature
  4. waitAfter about 30 min
  5. temperaturethe reaction mixture was warmed to about 80° C
  6. waitAfter about 30 min
  7. temperaturethe mixture was warmed to about 125° C
  8. waitAfter about 48 h
  9. temperatureto cool to ambient temperature
  10. customThe volatiles were removed under reduced pressure
  11. customThe residue was purified by silica gel chromatography
  12. washeluting with a gradient of 5-50% EtOAc in heptane

出典と根拠

ORDレコード
ord-9a3c0949a50c406ab1dbc7c9b7a0c678
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08426411B2

反応ノート

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