Triethylamine → {6-[2-(Tert-butyldimethylsilanyloxy)ethyl]-5-chloropyrazolo[1,5-a]pyrimidin-7-yl}[4-(2-methoxyethoxy)phenyl]amine

HRID 1452618노트

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HRID 1452618 반응식
[Si:1]([O:8][CH2:9][CH2:10][C:11]1[C:12]([Cl:21])=[N:13][C:14]2[N:15]([N:18]=[CH:19][CH:20]=2)[C:16]=1Cl)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C(N(CC)CC)C.[CH3:29][O:30][CH2:31][CH2:32][O:33][C:34]1[CH:39]=[CH:38][C:37]([NH2:40])=[CH:36][CH:35]=1>C(O)(C)C>[Si:1]([O:8][CH2:9][CH2:10][C:11]1[C:12]([Cl:21])=[N:13][C:14]2[N:15]([N:18]=[CH:19][CH:20]=2)[C:16]=1[NH:40][C:37]1[CH:36]=[CH:35][C:34]([O:33][CH2:32][CH2:31][O:30][CH3:29])=[CH:39][CH:38]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 38798854-(2-Methoxyethoxy)anilineHCID 575268026-[2-(Tert-butyldimethylsilanyloxy)ethyl]-5,7-dichloropyrazolo[1,5-a]pyrimidine

생성물 1

HCID 57526832{6-[2-(Tert-butyldimethylsilanyloxy)ethyl]-5-chloropyrazolo[1,5-a]pyrimidin-7-yl}[4-(2-methoxyethoxy)phenyl]amine

시약·촉매·용매 1

HCID 3776Isopropanol용매

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온도
85 °C

실험 절차

To an isopropanol (3.0 mL) solution containing 6-[2-(tert-butyldimethylsilanyloxy)ethyl]-5,7-dichloropyrazolo[1,5-a]pyrimidine (512 mg, 1.49 mmol), triethylamine (836 μL, 5.96 mmol) and 4-(2-methoxyethoxy)phenylamine (299 mg, 1.79 mmol) were added, and this mixture was heated at 85° C. with stirring. After the reaction, the solvent was concentrated, sodium hydrogen carbonate was added here, and the mixture was extracted with ethyl acetate. The combined ethyl acetate layer was dried over sodium sulfate. After the sodium sulfate was filtered off, the solvent was distilled off to obtain the title compound.

후처리

  1. additionwere added
  2. customAfter the reaction
  3. concentrationthe solvent was concentrated
  4. additionsodium hydrogen carbonate was added here
  5. extractionthe mixture was extracted with ethyl acetate
  6. dry with materialThe combined ethyl acetate layer was dried over sodium sulfate
  7. filtrationAfter the sodium sulfate was filtered off
  8. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-169e0f03092c424d989e41aede5430e9
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07473694B2

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