Ethyl Acetate → HCID 178419928, 화합물

HRID 2264209노트

반응식

HRID 2264209 반응식
[O:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]1[C:11]([C:12]2[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=2)=[CH:10][C:9]([NH2:18])=[C:8]([NH2:19])[N:7]=1.[CH2:20](OC(OCC)OCC)C.[OH-].[Na+].C(OCC)(=O)C>C(O)(=O)C>[O:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]1[N:7]=[C:8]2[NH:19][CH:20]=[N:18][C:9]2=[CH:10][C:11]=1[C:12]1[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 31214Ethyl orthoformateHCID 59595986HCID 59595986, 화합물2회

생성물 1

HCID 178419928HCID 178419928, 화합물수율 49%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
140 °C

실험 절차

A mixture of 2-(1,3-oxazol-2-yl)-3,4′-bipyridine-5,6-diamine (Intermediate 10, 0.100 g, 0.39 mmol) and triethylorthoformate (0.117 g, 0.79 mmol) in glacial acetic acid (2 mL) was heated in a sealed tube to 140° C. After stirring for 2 hours, the mixture was cooled and taken to pH 7 with 6N aqueous sodium hydroxide solution. Ethyl acetate was added to the mixture and, after stirring for 30 minutes, the separated solid was filtered, washed with diethyl ether and dried in vacuo to give the title compound (0.047 g, 49%) as an off-white solid.

후처리

  1. temperaturethe mixture was cooled
  2. stirringafter stirring for 30 minutes
  3. filtrationthe separated solid was filtered
  4. washwashed with diethyl ether
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-575934924e984483af34fa8dd6ef9788
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07855202B2

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