ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Pyridine → N-{3-[5-(2-amino-4-pyrimidinyl)-2-(1,1-dimethylethyl)-1,3-thiazol-4-yl]-2-fluorophenyl}-2-pyridinesulfonamide

HRID 239538
ノート
印刷プレビュー

反応式

HRID 239538 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[S:7]([O-:9])=[O:8].[Na+].ClN1C(=O)CCC1=O.S(Cl)(Cl)(=O)=O.[NH2:24][C:25]1[C:26]([F:47])=[C:27]([C:31]2[N:32]=[C:33]([C:43]([CH3:46])([CH3:45])[CH3:44])[S:34][C:35]=2[C:36]2[CH:41]=[CH:40][N:39]=[C:38]([NH2:42])[N:37]=2)[CH:28]=[CH:29][CH:30]=1.N1C=CC=CC=1>ClCCl>[NH2:42][C:38]1[N:37]=[C:36]([C:35]2[S:34][C:33]([C:43]([CH3:45])([CH3:46])[CH3:44])=[N:32][C:31]=2[C:27]2[C:26]([F:47])=[C:25]([NH:24][S:7]([C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=3)(=[O:9])=[O:8])[CH:30]=[CH:29][CH:28]=2)[CH:41]=[CH:40][N:39]=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 5

HCID 1049PyridineHCID 24648Sulfuryl chlorideHCID 31398ChlorosuccinimideHCID 23678794Sodium Pyridine-2-sulfinateHCID 579897094-[4-(3-Amino-2-fluorophenyl)-2-(1,1-dimethylethyl)-1,3-thiazol-5-yl]-2-pyrimidinamine

生成物 1

HCID 57989786
N-{3-[5-(2-amino-4-pyrimidinyl)-2-(1,1-dimethylethyl)-1,3-thiazol-4-yl]-2-fluorophenyl}-2-pyridinesulfonamide
収率 12.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a suspension of sodium 2-pyridinesulfinate (48.4 mg, 0.291 mmol) in dichloromethane (3 ml) was added N-chlorosuccinimide (38.9 mg, 0.291 mmol). After 1 hour, the reaction mixture was filtered through a short Celite plug. To the crude sulfonyl chloride solution was added the 4-[4-(3-amino-2-fluorophenyl)-2-(1,1-dimethylethyl)-1,3-thiazol-5-yl]-2-pyrimidinamine (50 mg, 0.146 mmol) and pyridine (0.035 ml, 0.437 mmol), and the mixture was stirred for 3 hours at ambient temperature. After 3 hours, the reaction was quenched with methanol, and the crude reaction mixture was concentrated, redissolved in methanol, and purified via reversed-phase HPLC chromatography, eluting with 30-60% acetonitrile/0.1% aqueous trifluoroacetic acid. The desired fractions were combined, neutralized with aqueous saturated sodium bicarbonate, and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated to obtain the title compound (8.8 mg, 12%) as tan solid. MS (ESI): 485 [M+H]+.

後処理

  1. filtrationthe reaction mixture was filtered through a short Celite plug
  2. waitAfter 3 hours
  3. customthe reaction was quenched with methanol
  4. customthe crude reaction mixture
  5. concentrationwas concentrated
  6. dissolutionredissolved in methanol
  7. custompurified via reversed-phase HPLC chromatography
  8. washeluting with 30-60% acetonitrile/0.1% aqueous trifluoroacetic acid
  9. extractionextracted with ethyl acetate
  10. washThe organic layer was washed with brine
  11. dry with materialdried over anhydrous sodium sulfate
  12. filtrationfiltered
  13. concentrationconcentrated

出典と根拠

ORDレコード
ord-2a76a60d308c48f0ab36e1985728c9f7
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08642759B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート