1,2-Dimethoxyethane → Ethanesulfonic acid [6-(2-hydroxy-ethoxy)-5-(2-methoxy-phenoxy)-[2,2]bipyrimidinyl-4-yl]-amide

HRID 2252728

반응식

HRID 2252728 반응식
CC(C)([O-])C.[K+].C[O:8][CH2:9][CH2:10][O:11]C.Cl[C:14]1[N:19]=[C:18]([C:20]2[N:25]=[CH:24][CH:23]=[CH:22][N:21]=2)[N:17]=[C:16]([NH:26][S:27]([CH2:30][CH3:31])(=[O:29])=[O:28])[C:15]=1[O:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=1[O:39][CH3:40]>C(O)CO>[OH:8][CH2:9][CH2:10][O:11][C:14]1[N:19]=[C:18]([C:20]2[N:25]=[CH:24][CH:23]=[CH:22][N:21]=2)[N:17]=[C:16]([NH:26][S:27]([CH2:30][CH3:31])(=[O:29])=[O:28])[C:15]=1[O:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=1[O:39][CH3:40]

참가 물질

5

반응물 3

HCID 80711,2-DimethoxyethaneHCID 23665647Potassium tert-butoxideHCID 59645271Ethanesulfonic acid [6-chloro-5-(2-methoxy-phenoxy)-[2,2']bipyrimidinyl-4-yl]-amide

생성물 1

HCID 59645268Ethanesulfonic acid [6-(2-hydroxy-ethoxy)-5-(2-methoxy-phenoxy)-[2,2]bipyrimidinyl-4-yl]-amide

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

반응 조건

온도
85 °C

실험 절차

To a solution of potassium tert.-butoxide (366.5 mg) in ethylene glycol (5 ml) was added 1,2-dimethoxy ethane (5 ml) and ethanesulfonic acid [6-chloro-5-(2-methoxy-phenoxy)-[2,2′]bipyrimidinyl-4-yl]-amide (420 mg). The reaction mixture was heated to 85° C. for 7 days, concentrated in vacuo, poured onto water, acidified by 2N HCl, and extracted with ethyl acetate. The combined organic extracts were dried over magnesium sulfate and concentrated in vacuo. The precipitated product was washed with diethyl ether, filtered and dried at HV to give ethanesulfonic acid [6-(2-hydroxy-ethoxy)-5-(2-methoxy-phenoxy)-[2,2′]bipyrimidinyl-4-yl]-amide (400 mg). LC-MS: tR: 3.45, [M+H]+: 448.24.

후처리

  1. concentrationconcentrated in vacuo
  2. additionpoured onto water
  3. extractionextracted with ethyl acetate
  4. dry with materialThe combined organic extracts were dried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. washThe precipitated product was washed with diethyl ether
  7. filtrationfiltered
  8. customdried at HV

출처 및 근거

ORD 기록
ord-daca05c35a284770ab324c5d6ee82d46
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07323465B2

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