Cyanoacetic acid → HCID 2799775, 화합물

HRID 1903099노트

반응식

HRID 1903099 반응식
[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]

참가 물질

5

반응물 3

HCID 9740Cyanoacetic acidHCID 10868DicyclohexylcarbodiimideHCID 195092-Pyridinemethanamine

생성물 1

HCID 2799775HCID 2799775, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매3회

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-f61fb57231064762a9e1ef3c7a1b6bf2
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04435407

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