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Ethanolamine → Ethanol, 2-[[2-amino-5-[(4-chlorophenyl)ethynyl]-4-pyrimidinyl]amino]-

HRID 1271032
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반응식

HRID 1271032 반응식
Cl[C:2]1[C:7]([C:8]#[C:9][C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)=[CH:6][N:5]=[C:4]([N:17]=CN(C(C)C)C(C)C)[N:3]=1.[CH2:26]([CH2:28][NH2:29])[OH:27]>C(O)C>[NH2:17][C:4]1[N:3]=[C:2]([NH:29][CH2:28][CH2:26][OH:27])[C:7]([C:8]#[C:9][C:10]2[CH:11]=[CH:12][C:13]([Cl:16])=[CH:14][CH:15]=2)=[CH:6][N:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 700EthanolamineHCID 734464494-Chloro-5-(4-chlorophenylethynyl)-2-diisopropylaminomethyleneaminopyrimidine

생성물 1

HCID 9857143Ethanol, 2-[[2-amino-5-[(4-chlorophenyl)ethynyl]-4-pyrimidinyl]amino]-

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 0.7 g of 4-chloro-5-(4-chlorophenylethynyl)-2-diisopropylaminomethyleneamino-pyrimidine, 20 mL ethanol and 0.6 mL ethanolamine was refluxed for 18 hours. The green solution was evaporated in vacuo and triturated with water. The insoluble yellow residue was recrystallized by dissolving in 35 mL hot methanol, concentrating to 10 mL and chilling. The pale yellow powdery precipitate was filtered and dried to yield 0.34 g of 2-amino-5-(4-chlorophenylethynyl)-4-(2-hyroxyethylamino)pyrimidine, m.p. 197–200° C.

후처리

  1. temperaturewas refluxed for 18 hours
  2. customThe green solution was evaporated in vacuo
  3. customtriturated with water
  4. customThe insoluble yellow residue was recrystallized
  5. dissolutionby dissolving in 35 mL hot methanol
  6. concentrationconcentrating to 10 mL
  7. temperaturechilling
  8. filtrationThe pale yellow powdery precipitate was filtered
  9. customdried

출처 및 근거

ORD 기록
ord-89b0b7b6b2dc4ca7aec700dedbfebed3
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07205297B2

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