Thiophosgene → 3-Isothiocyanato-4-methoxypyridine

HRID 405676

反応式

HRID 405676 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 866653953-Isothiocyanato-4-methoxypyridine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ee87ebf960e44ad2a380b9ee83717c12
出典データセット
uspto-grants-2014_06
特許番号
US08753857B2

関連ノート

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