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2-(Dimethylamino)ethanol → HCID 57690626、化合物

HRID 401502
ノート
印刷プレビュー

反応式

HRID 401502 の反応式
CN(C)CCO.[Li].[CH:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:11]=[C:10]([N:18]2[CH2:23][CH2:22][N:21]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:20][CH2:19]2)[N:9]=1.[F:31][C:32]1[N:43]=[CH:42][CH:41]=[CH:40][C:33]=1[C:34](N(OC)C)=[O:35]>C1COCC1>[F:31][C:32]1[N:43]=[CH:42][CH:41]=[CH:40][C:33]=1[C:34]([C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:11]=[C:10]([N:18]2[CH2:19][CH2:20][N:21]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:22][CH2:23]2)[N:9]=1)=[O:35]
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

6

反応物 4

HCID 79022-(Dimethylamino)ethanolHCID 3028194LithiumHCID 534170672-Fluoro-N-methoxy-N-methylnicotinamideHCID 57690803tert-Butyl 4-(isoquinolin-3-yl)piperazine-1-carboxylate

生成物 1

HCID 57690626HCID 57690626、化合物収率 8%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

反応条件

温度
-78 °C

実験手順

A solution of 2-dimethylaminoethanol (0.072 ml, 0.72 mmol) in hexanes (3 ml) was cooled down to −40° C. A 2.5M solution of nbutyl lithium in tetrahydrofuran (0.574 ml, 1.44 mmol) was added dropwise. The solution was stirred for 20 minutes. A suspension of tert-butyl 4-(isoquinolin-3-yl)piperazine-1-carboxylate (0.75 mg, 0.24 mmol) in hexanes (8 ml) was added and the resulting solution was stirred for 1 hour. The solution was cooled down to −78° C. A solution of 2-fluoro-N-methoxy-N-methylnicotinamide (176.3 mg, 0.96 mmol) in THF (40 ml) was added dropwise. The reaction mixture was warmed up to −50° and stirred for 1 hour, then the mixture was stirred at 0° C. for a further 1 hour. The crude mixture was partitioned between water and ethyl acetate. The organic extract was dried over magnesium sulfate, filtered and concentrated under vacuo. The residue was and purified on silica gel by flash column chromatography to give the title compound as a yellow oil (8 mg, 8% yield).

後処理

  1. additionwas added
  2. stirringthe resulting solution was stirred for 1 hour
  3. temperatureThe reaction mixture was warmed up to −50°
  4. stirringstirred for 1 hour
  5. stirringthe mixture was stirred at 0° C. for a further 1 hour
  6. customThe crude mixture was partitioned between water and ethyl acetate
  7. extractionThe organic extract
  8. dry with materialwas dried over magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated under vacuo
  11. custompurified on silica gel by flash column chromatography

出典と根拠

ORDレコード
ord-c1d12809e815467b9afc7a8a7d9b42db
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08741931B2

反応ノート

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