4-Amino-3-hydroxypyridine → 4-[[(1-Piperidinyl)methylene]amino]-3-pyridinol

HRID 362194

反応式

HRID 362194 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[OH:8].CO[C:11](OC)([N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1)N>>[N:13]1([CH:11]=[N:1][C:2]2[CH:7]=[CH:6][N:5]=[CH:4][C:3]=2[OH:8])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1

参加物

3

反応物 2

HCID 27624194-Amino-3-hydroxypyridineHCID 570644181-Piperidinylformamide dimethyl acetal

生成物 1

HCID 153809334-[[(1-Piperidinyl)methylene]amino]-3-pyridinol

反応条件

温度
100 °C

実験手順

4-Amino-3-pyridinol (3.3 g) was added to 1-piperidinylformamide dimethyl acetal (50 ml) and the mixture was stirred at 100° C. until it became homogeneous (approximately one minute). The reaction mixture was cooled, and placed in an ice bath for a half hour. The crystallized product was filtered, washed well with diethyl ether, and air dried to yield 4.64 g of product. This was recrystallized from ethyl acetate and dried under high vacuum and refluxing ethanol overnight to yield 3.39 g of fluffy needles, m.p. 171°-172.5° C.

後処理

  1. custom(approximately one minute)
  2. temperatureThe reaction mixture was cooled
  3. waitplaced in an ice bath for a half hour
  4. filtrationThe crystallized product was filtered
  5. washwashed well with diethyl ether, and air
  6. customdried

出典と根拠

ORDレコード
ord-3efc76301fb44042b4cd101b21943b90
出典データセット
uspto-grants-1999_02
特許番号
US05869480

関連ノート

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