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Water → HCID 86692512、化合物

HRID 1748566
ノート
印刷プレビュー

反応式

HRID 1748566 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH3:17])[C:5]([C:8]2(C(O)=O)[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)=[N:6][CH:7]=1.O>CS(C)=O>[Br:1][C:2]1[CH:3]=[C:4]([CH3:17])[C:5]([CH:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)=[N:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 962WaterHCID 86692511HCID 86692511、化合物

生成物 1

HCID 86692512HCID 86692512、化合物収率 88.2%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A solution of 4-(5-bromo-3-methylpyridin-2-yl)tetrahydro-2H-pyran-4-carboxylic acid (420 mg) in dimethylsulfoxide (1 ml) was stirred at 150° C. for 1.5 hours. After completion of the reaction, the mixture was cooled to room temperature, water was added thereto, and extracted with chloroform. The organic layer was washed with water and saturated brine sequentially, then dried over anhydrous sodium sulfate, and the solvent was evaporated. The obtained residue was purified with silica gel column chromatography (n-hexane/ethyl acetate) to give the titled compound (316 mg) as a white solid. MS (ESI) m/z: 256, 258 (M+H)+.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customAfter completion of the reaction
  2. extractionextracted with chloroform
  3. washThe organic layer was washed with water and saturated brine sequentially
  4. dry with materialdried over anhydrous sodium sulfate
  5. customthe solvent was evaporated
  6. customThe obtained residue was purified with silica gel column chromatography (n-hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-b4ba8f8339a44ed397218c7b2c647938
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09150555B2

反応ノート

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