Ethanolamine → HCID 53261242, 화합물

HRID 876143노트

반응식

HRID 876143 반응식
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([O:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[CH:11][CH:10]=2)[CH:3]=1.[CH2:22]([CH2:24][NH2:25])[OH:23].CCN(C(C)C)C(C)C>CCCCO>[O:15]([C:12]1[CH:13]=[CH:14][C:9]([NH:8][C:4]2[N:5]=[CH:6][N:7]=[C:2]([NH:25][CH2:24][CH2:22][OH:23])[CH:3]=2)=[CH:10][CH:11]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

5

반응물 3

HCID 700EthanolamineHCID 81531DiisopropylethylamineHCID 63549578HCID 63549578, 화합물

생성물 1

HCID 53261242HCID 53261242, 화합물수율 60%

시약·촉매·용매 1

HCID 2631-Butanol용매2회

반응 조건

온도
200 °C

실험 절차

225 mg of 6-chloro-N-(4-phenoxyphenyl)pyrimidin-4-amine, 82 mg of ethanolamine and 173 mg of DIPEA were dissolved in 2 mL of n-BuOH and the mixture obtained was charged into a microwave vial and the vial obtained was heated to 200° C. for 60 minutes under microwave irradiation. Progress of the reaction was monitored by TLC. Upon termination of the reaction n-BuOH was evaporated and the evaporation residue was subjected to MPLC purification (EtOAc:EtOH=10:1). 2-(6-(4-Phenoxyphenylamino)pyrimidin-4-ylamino)ethan-1-ol was obtained in the form of a colorless solid.

후처리

  1. customthe mixture obtained
  2. additionwas charged into a microwave vial
  3. customthe vial obtained
  4. customwas evaporated
  5. customthe evaporation residue was subjected to MPLC purification (EtOAc:EtOH=10:1)

출처 및 근거

ORD 기록
ord-a450df9566d5498ba2efb668d89e465f
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08986994B2

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