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tert-Butyl 4-oxopiperidine-1-carboxylate → HCID 58441736、化合物

HRID 2262146
ノート
印刷プレビュー

反応式

HRID 2262146 の反応式
[Cl:1][C:2]1[N:3]=[C:4]([N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[C:5]2[S:10][CH:9]=[CH:8][C:6]=2[N:7]=1.C([Li])CCC.[C:22]([N:29]1[CH2:34][CH2:33][C:32](=[O:35])[CH2:31][CH2:30]1)([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23]>O1CCCC1>[C:25]([O:24][C:22]([N:29]1[CH2:34][CH2:33][C:32]([C:9]2[S:10][C:5]3[C:4]([N:11]4[CH2:16][CH2:15][O:14][CH2:13][CH2:12]4)=[N:3][C:2]([Cl:1])=[N:7][C:6]=3[CH:8]=2)([OH:35])[CH2:31][CH2:30]1)=[O:23])([CH3:28])([CH3:26])[CH3:27]
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 735900tert-Butyl 4-oxopiperidine-1-carboxylateHCID 202849712-Chloro-4-(morpholin-4-yl)thieno(3,2-d)pyrimidineHCID 178418339Butyllithium

生成物 1

HCID 58441736HCID 58441736、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-40 °C

実験手順

To solution of 2-chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidine 4 (1.22 g) in anhydrous tetrahydrofuran (20 ml) stirring at −78° C. was added 2.5M n-butyllithium in hexanes (2.3 mL). The reaction mixture was warmed gradually to −40° C. over 1 hour, cooled to −78° C., and 1-BOC-4-Piperidone (950 mg) was added. The reaction mixture was gradually warmed to room temperature and then left to stir for 2 hours, poured into ice/water and extracted into ethyl acetate. After the usual drying and evaporation of the solvent, the residue was purified by flash chromatography to give 4-(2-chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidin-6-yl)-4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester.

後処理

  1. temperaturecooled to −78° C.
  2. temperatureThe reaction mixture was gradually warmed to room temperature
  3. waitleft
  4. extractionextracted into ethyl acetate
  5. customAfter the usual drying
  6. customevaporation of the solvent
  7. customthe residue was purified by flash chromatography

出典と根拠

ORDレコード
ord-2e7c3b962849450aa29fdad661c7300c
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07846929B2

反応ノート

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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