1-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-(2-methoxy-ethoxy)-1H-pyrrolo[2,3-c]pyridine-2-carboxylic acid ethyl ester → 1-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-(2-methoxy-ethoxy)-1H-pyrrolo[2,3-c]pyridine-2-carboxylic acid

HRID 2250440노트

반응식

HRID 2250440 반응식
C([O:3][C:4]([C:6]1[N:19]([CH2:20][C:21]2[CH:25]=[C:24]([C:26]3[S:27][C:28]([Cl:31])=[CH:29][CH:30]=3)[O:23][N:22]=2)[C:9]2=[CH:10][N:11]=[C:12]([O:14][CH2:15][CH2:16][O:17][CH3:18])[CH:13]=[C:8]2[CH:7]=1)=[O:5])C>C1COCC1.CO>[Cl:31][C:28]1[S:27][C:26]([C:24]2[O:23][N:22]=[C:21]([CH2:20][N:19]3[C:9]4=[CH:10][N:11]=[C:12]([O:14][CH2:15][CH2:16][O:17][CH3:18])[CH:13]=[C:8]4[CH:7]=[C:6]3[C:4]([OH:5])=[O:3])[CH:25]=2)=[CH:30][CH:29]=1

참가 물질

4

반응물 1

HCID 692251001-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-(2-methoxy-ethoxy)-1H-pyrrolo[2,3-c]pyridine-2-carboxylic acid ethyl ester

생성물 1

HCID 670112231-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-(2-methoxy-ethoxy)-1H-pyrrolo[2,3-c]pyridine-2-carboxylic acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

To a solution of 1.3 g (2.814 mmol) 1-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-(2-methoxy-ethoxy)-1H-pyrrolo[2,3-c]pyridine-2-carboxylic acid ethyl ester in 30 mL THF and 15 mL MeOH 11.26 mL 1M LiOH solution were added and the mixture was stirred at 50° C. for 3 h. The organic solvents were removed in vacuo, 50 mL of water were added and the pH was adjusted to pH 2 with 1N HCl solution. The desired product precipitated and was filtered, washed with water and dried over P2O5. Yield 1.11 g.

후처리

  1. customThe organic solvents were removed in vacuo, 50 mL of water
  2. additionwere added
  3. customThe desired product precipitated
  4. filtrationwas filtered
  5. washwashed with water
  6. dry with materialdried over P2O5

출처 및 근거

ORD 기록
ord-19f71d02c8dc44068a3879f400ebd557
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07317027B2

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