Chloroacetaldehyde → 6-Bromo-N-(2-thiazolyl)pyridin-2-amine

HRID 49140

반응식

HRID 49140 반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([NH:8][C:9]([NH2:11])=[S:10])[N:3]=1.Cl[CH2:13][CH:14]=O>C(O)C.O>[Br:1][C:2]1[N:3]=[C:4]([NH:8][C:9]2[S:10][CH:13]=[CH:14][N:11]=2)[CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 33ChloroacetaldehydeHCID 22170428(6-Bromo-pyridin-2-YL)thiourea

생성물 1

HCID 221704016-Bromo-N-(2-thiazolyl)pyridin-2-amine수율 96%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A suspension of 2-bromo-6-thioureidopyridine (3 g, 12.92 mmol) and chloroacetaldehyde (3.28 mL, 25.85 mmol) in ethanol (27 mL) and water (7 mL) was heated at reflux for 4.75 h. The solution was concentrated in vacuo and the residue was diluted with 1 N aqueous NaOH solution at 0° C., stirred for 10 min, and the pH was then adjusted to 8.5 by addition of 6 N aqueous HCl solution. The precipitate was collected by filtration, washed several times with water and dried in vacuo over P2O5 to obtain the titled compound (3.17 g, 96%) as a light yellow solid.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 4.75 h
  3. concentrationThe solution was concentrated in vacuo
  4. additionthe residue was diluted with 1 N aqueous NaOH solution at 0° C.
  5. additionthe pH was then adjusted to 8.5 by addition of 6 N aqueous HCl solution
  6. filtrationThe precipitate was collected by filtration
  7. washwashed several times with water
  8. dry with materialdried in vacuo over P2O5

출처 및 근거

ORD 기록
ord-6008bb2fbb9e4cdab9922f9daf64bc80
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706717B2

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