Water → HCID 57377894、化合物

HRID 72545ノート

反応式

HRID 72545 の反応式
[CH2:1]([CH:8]1[CH2:12][CH2:11][CH2:10][N:9]1[C:13]1[N:34]=[CH:33][C:32]([Cl:35])=[CH:31][C:14]=1[C:15]([NH:17][C:18]1([C:21]2[CH:30]=[CH:29][C:24]([C:25]([O:27]C)=[O:26])=[CH:23][CH:22]=2)[CH2:20][CH2:19]1)=[O:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O>O1CCOCC1>[CH2:1]([CH:8]1[CH2:12][CH2:11][CH2:10][N:9]1[C:13]1[N:34]=[CH:33][C:32]([Cl:35])=[CH:31][C:14]=1[C:15]([NH:17][C:18]1([C:21]2[CH:30]=[CH:29][C:24]([C:25]([OH:27])=[O:26])=[CH:23][CH:22]=2)[CH2:20][CH2:19]1)=[O:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 962WaterHCID 67958026Methyl 4-(1-(2-(2-benzylpyrrolidin-1-yl)-5-chloronicotinamido)cyclopropyl)benzoate

生成物 1

HCID 57377894HCID 57377894、化合物収率 80.9%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
150 °C

実験手順

To a solution of methyl 4-(1-(2-(2-benzylpyrrolidin-1-yl)-5-chloronicotinamido)cyclopropyl)benzoate (D144) (60 mg, 0.122 mmol) in 1,4-dioxane (3 ml) and water (1 ml) lithium hydroxide monohydrate (7.7 mg, 0.18 mmol) was added and the resulting mixture was stirred at 150° C. under microwave irradiation for 10 min (2 cycles of 5 min each). Solvents were evaporated in vacuo, and the residue was diluted with water (5 ml) and 1M HCl (15 ml) and extracted with ethylacetate (3×20 ml). Collected organics, after solvent evaporation, afforded the title compound (E7) (racemic mixture) (47 mg).

後処理

  1. customSolvents were evaporated in vacuo
  2. additionthe residue was diluted with water (5 ml) and 1M HCl (15 ml)
  3. extractionextracted with ethylacetate (3×20 ml)
  4. customCollected organics, after solvent evaporation

出典と根拠

ORDレコード
ord-adc2f430413e428db5d9cea33e87cffc
出典データセット
uspto-grants-2014_09
特許番号
US08828987B2

反応ノート

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