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

HRID 1452618ノート

反応式

HRID 1452618 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
85 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-169e0f03092c424d989e41aede5430e9
出典データセット
uspto-grants-2009_01
特許番号
US07473694B2

反応ノート

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