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Triethylamine → 1-(1,3-Dihydroisobenzofuran-5-yl)-N-(6'-methoxy-3,5'-dimethyl-2,3'-bipyridin-6-yl)cyclopropanecarboxamide

HRID 870010
ノート
印刷プレビュー

反応式

HRID 870010 の反応式
[CH2:1]1[C:9]2[C:4](=[CH:5][C:6]([C:10]3([C:13]([OH:15])=O)[CH2:12][CH2:11]3)=[CH:7][CH:8]=2)[CH2:3][O:2]1.S(Cl)(Cl)=O.[CH3:20][O:21][C:22]1[N:27]=[CH:26][C:25]([C:28]2[C:33]([CH3:34])=[CH:32][CH:31]=[C:30]([NH2:35])[N:29]=2)=[CH:24][C:23]=1[CH3:36].CCN(CC)CC>ClCCl.CN(C=O)C>[CH2:1]1[C:9]2[C:4](=[CH:5][C:6]([C:10]3([C:13]([NH:35][C:30]4[N:29]=[C:28]([C:25]5[CH:26]=[N:27][C:22]([O:21][CH3:20])=[C:23]([CH3:36])[CH:24]=5)[C:33]([CH3:34])=[CH:32][CH:31]=4)=[O:15])[CH2:11][CH2:12]3)=[CH:7][CH:8]=2)[CH2:3][O:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 59129550HCID 59129550、化合物HCID 68722468HCID 68722468、化合物

生成物 1

HCID 687244141-(1,3-Dihydroisobenzofuran-5-yl)-N-(6'-methoxy-3,5'-dimethyl-2,3'-bipyridin-6-yl)cyclopropanecarboxamide収率 48.1%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
触媒
HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 1-(1,3-dihydroisobenzofuran-5-yl)cyclopropanecarboxylic acid (40.8 mg, 0.2 mmol) in dichloromethane (2 mL) was added thionyl chloride (43.8 μL, 0.60 mmol) followed by DMF (1 drop) and the reaction was stirred at room temperature for 30 minutes and then the solvent was evaporated. Toluene (˜1 mL) was added and mixed with the residue and then removed by rotovap. The residue was then dissolved in dichloromethane (1 mL) and a solution of 6′-methoxy-3,5′-dimethyl-2,3′-bipyridin-6-amine (45.8 mg, 0.20 mmol) and Et3N (83.6 μL, 0.60 mmol) in dichloromethane (1 mL) was added. The reaction was stirred at room temperature for 12 hours. The reaction was then concentrated. The residue was dissolved in DMSO and purified by reverse phase HPLC (10-99% CH3CN in water) to yield 40 mg of the desired product. ESI-MS m/z calc. 415.2. found 416.5 (M+1)+. Retention time 1.87 minutes.

後処理

  1. customthe solvent was evaporated
  2. additionToluene (˜1 mL) was added
  3. additionmixed with the residue
  4. customremoved by rotovap
  5. dissolutionThe residue was then dissolved in dichloromethane (1 mL)
  6. stirringThe reaction was stirred at room temperature for 12 hours
  7. concentrationThe reaction was then concentrated
  8. dissolutionThe residue was dissolved in DMSO
  9. custompurified by reverse phase HPLC (10-99% CH3CN in water)

出典と根拠

ORDレコード
ord-0763fec9a8e941a089ec293e632b7fe8
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08969386B2

反応ノート

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