Thiophosgene → 3-Isothiocyanato-4-methoxypyridine

HRID 333589

반응식

HRID 333589 반응식
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[O:8][CH3:9].C([O-])(O)=O.[Na+].[C:15](Cl)(Cl)=[S:16]>C(Cl)(Cl)Cl.O>[N:1]([C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[O:8][CH3:9])=[C:15]=[S:16]

참가 물질

6

반응물 3

HCID 10040ThiophosgeneHCID 516892Sodium BicarbonateHCID 52003433-Amino-4-methoxypyridine

생성물 1

HCID 866653953-Isothiocyanato-4-methoxypyridine

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

To a stirred mixture of 3-amino-4-methoxypyridine (2.01 g, 16.2 mmol) and NaHCO3 (4.08 g, 48.6 mmol) in CHCl3 and water (1:1, 50 mL) at 4° C. was added thiophosgene (1.5 mL, 19.6 mmol) dropwise. After completion of the addition, the ice bath was removed. The mixture was stirred for 4 hours, the organic layer was separated, and the aqueous layer was extracted with CH2Cl2. The combined organic phases were washed with water, dried over Na2SO4, filtered, and concentrated to give the title compound as brown solid.

후처리

  1. additionAfter completion of the addition
  2. customthe ice bath was removed
  3. customthe organic layer was separated
  4. extractionthe aqueous layer was extracted with CH2Cl2
  5. washThe combined organic phases were washed with water
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-db54b7916c324950a910de618568492c
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883473B2

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