Morpholine → 4-(4-Bromo-1,3-thiazol-2-yl)morpholine

HRID 244486

反応式

HRID 244486 の反応式
Br[C:2]1[S:3][CH:4]=[C:5]([Br:7])[N:6]=1.[NH:8]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1>O>[Br:7][C:5]1[N:6]=[C:2]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[S:3][CH:4]=1

参加物

4

反応物 2

HCID 8083MorpholineHCID 27632972,4-Dibromo-1,3-thiazole

生成物 1

HCID 438110424-(4-Bromo-1,3-thiazol-2-yl)morpholine収率 89.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 2,4-dibromothiazole (500 mg, 2.06 mmol) in morpholine (4.0 mL, 22.3 mmol) was warmed at 50° C. in a sealed tube. After 16 hours, the mixture was cooled to room temperature, diluted with 20 mL of water and extracted with three 30 mL portions of diethyl ether. The combined organic layers was washed with five 30 mL portions of water, 30 mL of brine, dried over magnesium sulfate, filtered, and concentrated in vacuo. The residue was chromatographed over SiO2 using ethyl acetate in hexanes (0-30% gradient) to afford 458 mg (89%) of 4-(4-bromothiazol-2-yl)morpholine.

後処理

  1. extractionextracted with three 30 mL portions of diethyl ether
  2. washThe combined organic layers was washed with five 30 mL portions of water, 30 mL of brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was chromatographed over SiO2

出典と根拠

ORDレコード
ord-232160f89dfd47b7a44bd470fa2c75fb
出典データセット
uspto-grants-2014_02
特許番号
US08658637B2

関連ノート

読み込み中…