Pyridine → (5-Cyanopyridin-2-yl)(methyl)carbamic chloride

HRID 539582노트

반응식

HRID 539582 반응식
C(=O)(OC(Cl)(Cl)Cl)[O:2][C:3]([Cl:6])(Cl)Cl.N1C=CC=CC=1.[CH3:19][NH:20][C:21]1[CH:28]=[CH:27][C:24]([C:25]#[N:26])=[CH:23][N:22]=1>O1CCCC1>[C:25]([C:24]1[CH:27]=[CH:28][C:21]([N:20]([CH3:19])[C:3]([Cl:6])=[O:2])=[N:22][CH:23]=1)#[N:26]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 94429TriphosgeneHCID 178608996-(Methylamino)pyridine-3-carbonitrile

생성물 1

HCID 86720259(5-Cyanopyridin-2-yl)(methyl)carbamic chloride

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of bis(trichloromethyl) carbonate (50 mg, 0.17 mmol) in tetrahydrofuran (2.0 mL) was added pyridine (0.04 mL, 0.510 mmol) dropwise under ice-cooling. After stirring under ice-cooling for 30 min, 6-(methylamino)nicotinonitrile (68 mg, 0.510 mmol) was added and the mixture was stirred at room temperature for 2.5 hours. The precipitated solid was filtered off. The filtrate containing (5-cyanopyridin-2-yl)(methyl)carbamic chloride (I-28) was directly used for next step.

후처리

  1. temperaturecooling
  2. temperaturecooling for 30 min
  3. stirringthe mixture was stirred at room temperature for 2.5 hours
  4. filtrationThe precipitated solid was filtered off
  5. additionThe filtrate containing (5-cyanopyridin-2-yl)(methyl)carbamic chloride (I-28)

출처 및 근거

ORD 기록
ord-dae7440a6e7a4fee95adafc6f1c6a2f1
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871754B2

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