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Sodium Hydroxide → (6-bromo-pyridin-3-ylmethyl)-[5-(5-chloro-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-pyridin-2-yl]-amine

HRID 509969
ノート
印刷プレビュー

反応式

HRID 509969 の反応式
C1(S([N:10]2[C:14]3=[N:15][CH:16]=[C:17]([Cl:19])[CH:18]=[C:13]3[C:12]([CH2:20][C:21]3[CH:22]=[CH:23][C:24]([NH2:27])=[N:25][CH:26]=3)=[CH:11]2)(=O)=O)C=CC=CC=1.[Br:28][C:29]1[N:34]=[CH:33][C:32]([CH:35]=O)=[CH:31][CH:30]=1.C([BH3-])#N.[OH-].[Na+].[Cl-].[NH4+]>C(O)C.C(O)(=O)C>[Br:28][C:29]1[N:34]=[CH:33][C:32]([CH2:35][NH:27][C:24]2[CH:23]=[CH:22][C:21]([CH2:20][C:12]3[C:13]4[C:14](=[N:15][CH:16]=[C:17]([Cl:19])[CH:18]=4)[NH:10][CH:11]=3)=[CH:26][N:25]=2)=[CH:31][CH:30]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 498716Cyano-borohydrideHCID 117692346-Bromo-3-pyridinecarboxaldehydeHCID 576192232-Pyridinamine, 5-[[5-chloro-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridin-3-yl]methyl]-

生成物 1

HCID 86653328
(6-bromo-pyridin-3-ylmethyl)-[5-(5-chloro-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-pyridin-2-yl]-amine
収率 31%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒

反応条件

温度
110 °C

実験手順

To 5-(1-benzenesulfonyl-5-chloro-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-pyridin-2-ylamine (120, 80.0 mg, 0.200 mmol) in 2.00 mL of ethanol and 0.10 mL of acetic acid, 6-bromo-pyridine-3-carbaldehyde (121, 100.0 mg, 0.538 mmol) and silica supported cyanoborohydride (0.50 g, 1.21 mmol/g) were added. The reaction was heated at 110° C. for 25 minutes in microwave. Sodium hydroxide (2.0 mL, 6.0 M aqueous) was added and the reaction heated at 100° C. for 10 minutes in microwave, then poured into aqueous ammonium chloride and extracted with ethyl acetate. The organic layer was separated, dried over sodium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material was purified by silica gel column chromatography eluting with 20% ethyl acetate in hexane. Appropriate fractions were combined and the solvent removed under vacuum to provide the desired compound (P-2002, 26.6 mg). MS (ESI) [M+H+]+=427.7, 429.7.

後処理

  1. additionwere added
  2. temperaturethe reaction heated at 100° C. for 10 minutes in microwave
  3. extractionextracted with ethyl acetate
  4. customThe organic layer was separated
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate concentrated under vacuum
  8. customThe resulting material was purified by silica gel column chromatography
  9. washeluting with 20% ethyl acetate in hexane
  10. customthe solvent removed under vacuum

出典と根拠

ORDレコード
ord-a7c0f1cb83b540849955abb66db96789
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096593B2

反応ノート

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