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

HRID 244486

반응식

HRID 244486 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-232160f89dfd47b7a44bd470fa2c75fb
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658637B2

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