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HCID 21490888、化合物 → HCID 21490910、化合物

HRID 1973904
ノート
印刷プレビュー

反応式

HRID 1973904 の反応式
[C:1]([C:4]1[CH:9]=[C:8]([NH2:10])[C:7]([CH2:11][CH2:12][CH2:13][CH3:14])=[C:6](Cl)[N:5]=1)(=[O:3])[NH2:2].C(C1C=C(Cl)C(CCCC)=C(N)N=1)(=O)N.[H][H]>CO.[Pd]>[C:1]([C:4]1[CH:9]=[C:8]([NH2:10])[C:7]([CH2:11][CH2:12][CH2:13][CH3:14])=[CH:6][N:5]=1)(=[O:3])[NH2:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 21490888HCID 21490888、化合物HCID 21490889HCID 21490889、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 21490910HCID 21490910、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

11.4 g (0.05 mol) of the isomer mixture of 2-carbamoyl-4-amino-5-n-butyl-6-chloro-pyridine and 2-carbamoyl-4-chloro-5-n-butyl-6-amino-pyridine, dissolved in 120 ml of pure methanol, are hydrogenated in the presence of 1.5 g of palladium on charcoal. After the calculated amount of hydrogen has been taken up, the catalyst is filtered off and the filtrate is evaporated to dryness. The residue is rendered alkaline with 2 N sodium carbonate solution and extracted with ether. The crystalline product which is soluble in neither sodium carbonate solution nor in ether is filtered off and rinsed with water. The white crystals are dried for 20 hours at 70° in a high vacuum. 2-Carbamoyl-4-amino-5-n-butyl-pyridine of the formula ##STR33## and of melting point 186°-190° is thus obtained.

後処理

  1. filtrationthe catalyst is filtered off
  2. customthe filtrate is evaporated to dryness
  3. extractionextracted with ether
  4. filtrationis filtered off
  5. washrinsed with water
  6. customThe white crystals are dried for 20 hours at 70° in a high vacuum

出典と根拠

ORDレコード
ord-edda81be66b0466e8efbc3d7a765f108
出典データセット
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03998955

反応ノート

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