4-Amino-3-hydroxypyridine → N,N-Diethyl-N'-(3-hydroxypyridin-4-yl)methanimidamide

HRID 361325

反応式

HRID 361325 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[OH:8].CO[CH:11](OC)[N:12]([CH2:15][CH3:16])[CH2:13][CH3:14]>C1(C)C=CC=CC=1>[CH2:13]([N:12]([CH:11]=[N:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[OH:8])[CH2:15][CH3:16])[CH3:14]

参加物

4

反応物 2

HCID 27624194-Amino-3-hydroxypyridineHCID 12747026N-(Dimethoxymethyl)-N-ethylethanamine

生成物 1

HCID 15380930N,N-Diethyl-N'-(3-hydroxypyridin-4-yl)methanimidamide収率 61.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 4-amino-3-pyridinol (3.90 g), N,N-diethylformamide dimethyl acetal (11.68 g) and toluene (20 mL) was heated under nitrogen for 2 hours. The solution was concentrated under reduced pressure. The resulting liquid was filtered through silica gel with 10% ethanol in tetrahydrofuran to give a solid. Recrystallization of the purified product from ethyl acetate/hexanes afforded 4.21 g of crystalline solid, m.p. 104°-106° C.

後処理

  1. temperaturewas heated under nitrogen for 2 hours
  2. concentrationThe solution was concentrated under reduced pressure
  3. filtrationThe resulting liquid was filtered through silica gel with 10% ethanol in tetrahydrofuran
  4. customto give a solid
  5. customRecrystallization of the purified product from ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-6b1219aad9914c19b842337f3fe8b169
出典データセット
uspto-grants-1999_02
特許番号
US05866565

関連ノート

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