Thiourea → HCID 58442446, 화합물

HRID 1843735노트

반응식

HRID 1843735 반응식
Br.Br[CH2:3][C:4]([C:6]1[C:7]([CH3:14])=[N:8][C:9]([CH3:13])=[CH:10][C:11]=1[CH3:12])=O.[NH2:15][C:16]([NH2:18])=[S:17]>CCO>[CH3:14][C:7]1[C:6]([C:4]2[N:15]=[C:16]([NH2:18])[S:17][CH:3]=2)=[C:11]([CH3:12])[CH:10]=[C:9]([CH3:13])[N:8]=1

참가 물질

4

반응물 2

HCID 2723790ThioureaHCID 86657727HCID 86657727, 화합물

생성물 1

HCID 58442446HCID 58442446, 화합물수율 62.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 2-bromo-1-(2,4,6-trimethylpyridin-3-yl)ethanone hydrobromide (9.00 g, 27.9 mmol) and thiourea (2.12 g, 27.9 mmol) in 95% EtOH (39.8 mL) was heated at reflux for 120 min. The solution was concentrated and added with water (50 mL) and saturated aqueous Na2CO3 (5.0 mL). The resultant precipitate was filtered and recrystallized in toluene. The solids were filtered and dried under vacuum to give 4-(2,4,6-trimethylpyridin-3-yl)thiazol-2-amine (3.80 g) as yellow solids in 62% yield: 1H NMR (500 MHz, CDCl3) δ 6.87 (s, 1 H), 6.31 (s, 1 H), 5.07 (bs, 2 H), 2.49 (s, 3 H), 2.38 (s, 3 H), 2.14 (s, 3 H).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 120 min
  3. concentrationThe solution was concentrated
  4. additionadded with water (50 mL) and saturated aqueous Na2CO3 (5.0 mL)
  5. filtrationThe resultant precipitate was filtered
  6. customrecrystallized in toluene
  7. filtrationThe solids were filtered
  8. customdried under vacuum

출처 및 근거

ORD 기록
ord-9cb6c34c3c6b4cc7b9e85cdaddb2e36c
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946268B2

반응 노트

불러오는 중…