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Potassium Carbonate → 4-(2-Butynyloxy)-6-(3,3-dimethylpiperidino)pyrimidine

HRID 2076867
ノート
印刷プレビュー

反応式

HRID 2076867 の反応式
[CH2:1]([O:5][C:6]1[CH:11]=[C:10](Cl)[N:9]=[CH:8][N:7]=1)[C:2]#[C:3][CH3:4].C(=O)([O-])[O-].[K+].[K+].Cl.[CH3:20][C:21]1([CH3:27])[CH2:26][CH2:25][CH2:24][NH:23][CH2:22]1.[Cl-].[NH4+]>C(#N)C>[CH2:1]([O:5][C:6]1[CH:11]=[C:10]([N:23]2[CH2:24][CH2:25][CH2:26][C:21]([CH3:27])([CH3:20])[CH2:22]2)[N:9]=[CH:8][N:7]=1)[C:2]#[C:3][CH3:4]
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 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 121376024-(2-Butynyloxy)-6-chloropyrimidineHCID 186866273,3-Dimethylpiperidine hydrochloride

生成物 1

HCID 593411324-(2-Butynyloxy)-6-(3,3-dimethylpiperidino)pyrimidine収率 95.1%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

反応条件

温度
80 °C

実験手順

Into 2 ml of acetonitrile were added 0.20 g of 4-(2-butynyloxy)-6-chloropyrimidine, 0.45 g of potassium carbonate and 0.20 g of 3,3-dimethylpiperidine hydrochloride, and the mixture was stirred for 2 hours at 80° C. The reaction mixture was cooled to near room temperature, a saturated ammonium chloride aqueous solution was added therein, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.27 g of 4-(2-butynyloxy)-6-(3,3-dimethylpiperidino)pyrimidine (hereinafter, referred to as Compound (31)).

後処理

  1. temperatureThe reaction mixture was cooled to near room temperature
  2. extractionthe mixture was extracted with tert-butyl methyl ether three times
  3. washThe organic layers were washed with a saturated sodium chloride aqueous solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-936a6b4da699458a9f984d36ca5096a6
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07928110B2

反応ノート

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