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

HRID 539582ノート

反応式

HRID 539582 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-dae7440a6e7a4fee95adafc6f1c6a2f1
出典データセット
uspto-grants-2014_10
特許番号
US08871754B2

反応ノート

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