Diglycolamine → 2-Amino-4-[2-(2-hydroxyethoxy)ethylamino]-5-phenylethynyl pyrimidine

HRID 1271036

반응식

HRID 1271036 반응식
Cl[C:2]1[C:7]([C:8]#[C:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:6][N:5]=[C:4]([N:16]=CN(C(C)C)C(C)C)[N:3]=1.[NH2:25][CH2:26][CH2:27][O:28][CH2:29][CH2:30][OH:31]>C(O)C>[NH2:16][C:4]1[N:3]=[C:2]([NH:25][CH2:26][CH2:27][O:28][CH2:29][CH2:30][OH:31])[C:7]([C:8]#[C:9][C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)=[CH:6][N:5]=1

참가 물질

4

반응물 2

HCID 13578DiglycolamineHCID 734464524-Chloro-2-diisopropylaminomethyleneamino-5-phenylethynylpyrimidine

생성물 1

HCID 98574242-Amino-4-[2-(2-hydroxyethoxy)ethylamino]-5-phenylethynyl pyrimidine수율 37.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1.5 g of 4-chloro-2-diisopropylaminomethyleneamino-5-phenylethynylpyrimidine, 20 mL of ethanol and 1.83 g of 2-(2-aminoethoxy)ethanol was refluxed for 18 hours. The tea colored solution was evaporated in vacuo and the residue partitioned between water and dichloromethane. The aqueous layer was washed twice more with dichloromethane and the combined organic extracts washed with water. The organic solution was dried over sodium sulfate, filtered and evaporated in vacuo. The yellow residue obtained was triturated with ether and filtered to give 0.49 g of a yellow solid, 2-amino-4-[2-(2-hydroxyethoxy)ethylamino]-5-phenylethynylpyrimidine. m.p. 128–129° C.

후처리

  1. temperaturewas refluxed for 18 hours
  2. customThe tea colored solution was evaporated in vacuo
  3. customthe residue partitioned between water and dichloromethane
  4. washThe aqueous layer was washed twice more with dichloromethane
  5. washthe combined organic extracts washed with water
  6. dry with materialThe organic solution was dried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated in vacuo
  9. customThe yellow residue obtained
  10. customwas triturated with ether
  11. filtrationfiltered

출처 및 근거

ORD 기록
ord-fb1d7b06e0004458b46d0c6a48157306
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07205297B2

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