Thionyl Chloride → HCID 178458779, 화합물

HRID 2236538노트

반응식

HRID 2236538 반응식
O[CH2:2][C:3]1[CH:8]=[C:7]([OH:9])[C:6]([O:10][CH2:11][CH2:12][CH3:13])=[CH:5][N:4]=1.S(Cl)([Cl:16])=O>C(Cl)(Cl)Cl>[Cl:16][CH2:2][C:3]1[CH:8]=[C:7]([OH:9])[C:6]([O:10][CH2:11][CH2:12][CH3:13])=[CH:5][N:4]=1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 178458791HCID 178458791, 화합물

생성물 1

HCID 178458779HCID 178458779, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a mixture of 2-hydroxymethyl-5-propoxy-pyridin-4-ol (5.56 g, 30.3 mmole) and 30 mL of chloroform stirred cooled with an ice bath is added 30 mL of thionyl chloride (x g, 0.x mole). This is stirred for 15 minutes at ice bath temperature and then refluxed for 1 hour. The reaction mixture is cooled, evaporated to dryness in vacuo and then treated with isopropanol. The solid is filtered, washed with fresh isopropanol, then ether and air dried to give an off-white solid, 3.4 g, (48%), m.p. 165-7° C.; MS (ES+): m/z 202.3 (M+H).

후처리

  1. temperaturecooled with an ice bath
  2. stirringThis is stirred for 15 minutes at ice bath temperature
  3. temperaturerefluxed for 1 hour
  4. temperatureThe reaction mixture is cooled
  5. customevaporated to dryness in vacuo
  6. additiontreated with isopropanol
  7. filtrationThe solid is filtered
  8. washwashed with fresh isopropanol
  9. dry with materialether and air dried
  10. customto give an off-white solid, 3.4 g, (48%), m.p. 165-7° C.

출처 및 근거

ORD 기록
ord-66f1ec9bb0884da8a56ede6feae45b90
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713994B2

반응 노트

불러오는 중…