3-(Chloromethyl)pyridine → HCID 22320205、化合物

HRID 498005

反応式

HRID 498005 の反応式
O=[C:2]([CH3:15])[CH2:3][C:4]1[O:9][C:8](=[O:10])[C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[N:5]=1.[NH:16]([CH2:18][C:19]1[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=1)[NH2:17].ClCC1C=NC=CC=1>C(O)C>[CH3:15][C:2]1[CH:3]=[C:4]([NH:5][C:6]2[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=2[C:8]([OH:9])=[O:10])[N:16]([CH2:18][C:19]2[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=2)[N:17]=1

参加物

5

反応物 3

HCID 183583-(Chloromethyl)pyridineHCID 12232495Pyridin-3-ylmethyl-hydrazineHCID 159380972-(2-Oxo-propyl)-benzo[D][1,3]oxazin-4-one

生成物 1

HCID 22320205HCID 22320205、化合物収率 67%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution in ethanol (50 mL) of 2-(2-oxopropyl)-4H-3,1-benzoxazin-4-one (11.2 g, 55.1 mmol) and 3-hydrazinomethylpyridine (7.44 g, 60.4 mmol) which was prepared from 3-chloromethylpyridine following the method described in Reference Example 2-2, was heated under reflux for 1 hour. The solution was cooled to room temperature, and the resulting crude crystals were collected by filtration. The crystals were washed with ethanol and air dried to give the title compound (11.3 g, 67% yield). mp: 180-183° C. (recrystallized from ethanol).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hour
  3. filtrationthe resulting crude crystals were collected by filtration
  4. washThe crystals were washed with ethanol and air
  5. customdried

出典と根拠

ORDレコード
ord-cf44457fb6344e3fba6132667320dab9
出典データセット
uspto-grants-2005_09
特許番号
US06949648B2

関連ノート

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