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Ethanolamine → HCID 72709697, 화합물

HRID 633763
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HRID 633763 반응식
Cl[C:2]1[N:7]=[CH:6][C:5]([C:8](=[O:32])[CH2:9][N:10]2[C:15]3=[N:16][C:17]([N:21]4[CH2:26][C@@H:25]5[CH2:27][C@H:22]4[CH2:23][O:24]5)=[CH:18][C:19](=[O:20])[N:14]3[CH2:13][CH2:12][C@H:11]2[C:28]([F:31])([F:30])[F:29])=[CH:4][CH:3]=1.[CH2:33]([CH2:35][NH2:36])[OH:34]>C(O)C>[OH:34][CH2:33][CH2:35][NH:36][C:2]1[N:7]=[CH:6][C:5]([C:8](=[O:32])[CH2:9][N:10]2[C:15]3=[N:16][C:17]([N:21]4[CH2:26][C@@H:25]5[CH2:27][C@H:22]4[CH2:23][O:24]5)=[CH:18][C:19](=[O:20])[N:14]3[CH2:13][CH2:12][C@H:11]2[C:28]([F:31])([F:30])[F:29])=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 700EthanolamineHCID 118194435HCID 118194435, 화합물

생성물 1

HCID 72709697HCID 72709697, 화합물수율 49.1%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
130 °C

실험 절차

A mixture of 0.50 mL of ethanol, 33 mg (0.070 mmol) of (8S)-9-[2-(6-chloropyrid-3-yl)-2-oxoethyl]-2-(1S,4S)-2-oxa-5-azabicyclo[2.2.1]hept-5-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one and 21.41 μl (0.352 mmol) of ethanolamine is heated in a Biotage microwave reactor at 130° C. for 30 minutes. The reaction mixture is evaporated to dryness and the residue is then taken up in 10 mL of water. The precipitate is filtered off and then dried under vacuum. 17 mg of (8S)-9-{2-[6-(2-hydroxyethylamino)pyrid-3-yl]-2-oxoethyl}-2-(1S,4S)-2-oxa-5-azabicyclo[2.2.1]hept-5-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one are obtained, the characteristics of which are as follows:

후처리

  1. customThe reaction mixture is evaporated to dryness
  2. filtrationThe precipitate is filtered off
  3. customdried under vacuum

출처 및 근거

ORD 기록
ord-14f00b118bb546529268d55a29f431e3
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321790B2

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