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Methylamine → 3-{[3-{[(5-Chloro-2-thienyl)sulfonyl]amino}-4-(methyloxy)-1H-indazol-1-yl]methyl}-N-methylbenzamide

HRID 1808622
ノート
印刷プレビュー

反応式

HRID 1808622 の反応式
[Cl:1][C:2]1[S:6][C:5]([S:7]([N:10](COCC[Si](C)(C)C)[C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][C:18]=3[O:20][CH3:21])[N:13]([CH2:22][C:23]3[CH:24]=[C:25]([CH:30]=[CH:31][CH:32]=3)[C:26]([O:28]C)=O)[N:12]=2)(=[O:9])=[O:8])=[CH:4][CH:3]=1.[NH:41]1CCCN2CCCN=[C:42]12.CN.CCCC[N+](CCCC)(CCCC)CCCC.[F-]>C1COCC1.C(Cl)Cl.O>[Cl:1][C:2]1[S:6][C:5]([S:7]([NH:10][C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][C:18]=3[O:20][CH3:21])[N:13]([CH2:22][C:23]3[CH:24]=[C:25]([CH:30]=[CH:31][CH:32]=3)[C:26]([NH:41][CH3:42])=[O:28])[N:12]=2)(=[O:8])=[O:9])=[CH:4][CH:3]=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 4

HCID 6329MethylamineHCID 79873TriazabicyclodeceneHCID 2724141Tetrabutylammonium FluorideHCID 58054540Methyl 3-{[3-[[(5-chloro-2-thienyl)sulfonyl]({[2-(trimethylsilyl)ethyl]oxy}methyl)amino]-4-(methyloxy)-1H-indazol-1-yl]methyl}benzoate

生成物 1

HCID 580545323-{[3-{[(5-Chloro-2-thienyl)sulfonyl]amino}-4-(methyloxy)-1H-indazol-1-yl]methyl}-N-methylbenzamide
収率 75%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
110 °C

実験手順

Methyl 3-{[3-[[(5-chloro-2-thienyl)sulfonyl]({[2-(trimethylsilyl)ethyl]oxy}methyl)amino]-4-(methyloxy)-1H-indazol-1-yl]methyl}benzoate (for a preparation see Intermediate 31) (70 mg, 0.112 mmol) in a Biotage microwave vial was added 1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidine (Aldrich) (7.83 mg, 0.056 mmol) and methylamine solution in THF (2M, 1.125 mL). The reaction vessel was sealed and heated in a Biotage Initiator microwave oven using initial very high absorption level to 80° C. for 75 min. The reaction mixture was diluted with DCM (2 mL) and water (3 mL). The organic phase was separated, and the aqueous layer was further extracted with DCM (2 mL). The combined organic solutions were dried through an hydrophobic frit and concentrated under a nitrogen stream in a blowdown unit. The residue was treated TBAF in THF (1M, 1.125 mL, 1.125 mmol). The reaction vessel was sealed and heated in a Biotage Initiator at 110° C. for 15 min (very high absorption level). The solvent was removed under a nitrogen stream in a blowdown unit (T=35° C. overnight), dissolved in 1:1 MeOH-DMSO (2 mL) and purified by Mass Directed AutoPrep on standard C18 column using Acetonitrile Water with a TFA modifier (Method B). The solvent was removed under a stream of nitrogen in a Radleys blowdown apparatus to give the title compound (41.7 mg, 75%) LCMS (System A) RT=1.03 min, ES+ve m/z 491/493 (M+H)+.

後処理

  1. customThe reaction vessel was sealed
  2. temperatureheated in a Biotage Initiator microwave oven
  3. customto 80° C.
  4. customfor 75 min
  5. customThe organic phase was separated
  6. extractionthe aqueous layer was further extracted with DCM (2 mL)
  7. customThe combined organic solutions were dried through an hydrophobic frit
  8. concentrationconcentrated under a nitrogen stream in a blowdown unit
  9. customThe reaction vessel was sealed
  10. customThe solvent was removed under a nitrogen stream in a blowdown unit (T=35° C. overnight)
  11. dissolutiondissolved in 1:1 MeOH-DMSO (2 mL)
  12. custompurified by Mass Directed AutoPrep on standard C18 column
  13. customThe solvent was removed under a stream of nitrogen in a Radleys blowdown apparatus

出典と根拠

ORDレコード
ord-0b815fb3d505437c938a46ded1239a3a
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08357716B2

反応ノート

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