3-(Chloromethyl)pyridine → HCID 22320205, 화합물

HRID 498005

반응식

HRID 498005 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 22320205HCID 22320205, 화합물수율 67%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-cf44457fb6344e3fba6132667320dab9
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949648B2

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