Cyanoacetic acid → HCID 2799775、化合物

HRID 1903099ノート

反応式

HRID 1903099 の反応式
[C:1]([CH2:3][C:4]([OH:6])=O)#[N:2].[NH2:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1.C1(N=C=NC2CCCCC2)CCCCC1>C(#N)C>[C:1]([CH2:3][C:4]([NH:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1)=[O:6])#[N:2]

参加物

5

反応物 3

HCID 9740Cyanoacetic acidHCID 10868DicyclohexylcarbodiimideHCID 195092-Pyridinemethanamine

生成物 1

HCID 2799775HCID 2799775、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒3 回

実験手順

To a solution of 6.8 g of cyanoacetic acid in 200 ml of acetonitrile was added a solution of 8.65 g of 2-aminomethylpyridine in 50 ml of acetonitrile, and to the resulting suspension there was added rapidly (with stirring) a solution of 18.5 g of dicyclohexylcarbodiimide in 50 ml of acetonitrile. After stirring 5 hours and standing overnight, the suspension was filtered. The filtrate was evaporated, and the crude residue was triturated with ether-ethyl acetate to give crystals, m.p. 78°-80°. Recrystallization from toluene yielded the 2-(cyanoacetylaminomethyl)-pyridine, m.p. 81°-82°.

後処理

  1. additionto the resulting suspension there was added rapidly
  2. waitstanding overnight
  3. filtrationthe suspension was filtered
  4. customThe filtrate was evaporated
  5. customthe crude residue was triturated with ether-ethyl acetate
  6. customto give crystals, m.p. 78°-80°
  7. customRecrystallization from toluene

出典と根拠

ORDレコード
ord-f61fb57231064762a9e1ef3c7a1b6bf2
出典データセット
uspto-grants-1984_03
特許番号
US04435407

反応ノート

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