Tetrahydrofuran → 1-(5-Bromo-3-phenoxypyridin-2-yl)thiourea

HRID 1809547노트

반응식

HRID 1809547 반응식
C([NH:9][C:10]([NH:12][C:13]1[C:18]([O:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[CH:17][C:16]([Br:26])=[CH:15][N:14]=1)=[S:11])(=O)C1C=CC=CC=1.C1COCC1.[OH-].[Na+]>O>[Br:26][C:16]1[CH:17]=[C:18]([O:19][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[C:13]([NH:12][C:10]([NH2:9])=[S:11])=[N:14][CH:15]=1

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 866410871-Benzoyl-3-(5-bromo-3-phenoxypyridin-2-yl)thiourea

생성물 1

HCID 866314811-(5-Bromo-3-phenoxypyridin-2-yl)thiourea수율 93%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A 2 L flask was charged with 1-benzoyl-3-(5-bromo-3-phenoxypyridin-2-yl)thiourea (94.3 g, 220 mmol) and THF (900 mL). 2M NaOH (330 mL, 660 mmol) was added and the reaction was heated at reflux overnight. The reaction was cooled to ambient temperature and 300 mL water was added slowly and then the THF was removed in vacuo to afford an aqueous slurry which was filtered, washed with water and dried to give 1-(5-bromo-3-phenoxypyridin-2-yl)thiourea (66.35 g, 93% yield) as a light tan solid.

후처리

  1. temperaturethe reaction was heated
  2. temperatureat reflux overnight
  3. customthe THF was removed in vacuo
  4. customto afford an aqueous slurry which
  5. filtrationwas filtered
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-2c4d19d8b65c41a587ecdfe6098d4560
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362037B2

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