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Tetrahydrofuran → Ethyl5-((1R)-1-{[(R)-tert-butylsulfinyl]amino}ethyl)-2-[(methylsulfonyl)amino]benzoate

HRID 1438385
ノート
印刷プレビュー

反応式

HRID 1438385 の反応式
[C:1]([C:4]1[CH:5]=[CH:6][C:7]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[C:8]([CH:13]=1)[C:9]([O:11][CH3:12])=[O:10])(=O)[CH3:2].[CH3:19][C:20]([S@:23]([NH2:25])=[O:24])([CH3:22])[CH3:21].[BH4-].[Na+].[CH2:28]1COCC1>[O-]CC.[Ti+4].[O-]CC.[O-]CC.[O-]CC>[C:20]([S@:23]([NH:25][C@@H:1]([C:4]1[CH:5]=[CH:6][C:7]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[C:8]([CH:13]=1)[C:9]([O:11][CH2:12][CH3:28])=[O:10])[CH3:2])=[O:24])([CH3:22])([CH3:21])[CH3:19]
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

6

反応物 4

HCID 8028TetrahydrofuranHCID 4311764Sodium borohydrideHCID 10964479tert-Butylsulfinamide, (R)-(+)-HCID 66978055Methyl 5-acetyl-2-[(methylsulfonyl)amino]benzoate

生成物 1

HCID 57762930Ethyl5-((1R)-1-{[(R)-tert-butylsulfinyl]amino}ethyl)-2-[(methylsulfonyl)amino]benzoate収率 23%

試薬・触媒・溶媒 1

HCID 76524
Titanium tetraethoxide
触媒

反応条件

温度
80 °C

実験手順

To a mixture of methyl 5-acetyl-2-[(methylsulfonyl)amino]benzoate (13.2 g, 49 mmol, PCT Int. Appl. WO2005003084), titanium (IV) ethoxide (100 ml) and THF (100 ml) was added (R)-(+)-2-methylpropane-2-sulfinamide (5.9 g, 49 mmol, Advanced Asymmmetry) and the mixture was stirred for 16 hours at 80° C. The mixture was cooled to room temperature and then to 0° C. before it was added dropwise into a 0° C. solution of sodium borohydride (7.4 g, 195 mmol). The mixture was stirred at 0° C. for 3 hours and then warmed to room temperature. The reaction was quenched with MeOH and stirred for 30 minutes. Then to the mixuture water was added. After stirring for 10 minutes, the resulting suspension was filtered through a celite pad and the filtered cake was washed with EtOAc. The filtrate was concentrated under reduced pressure to give a residue, which was applied to a silica gel chromatography column and eluted with a volume mixture of DCM and EtOAc (1/1) to afford 4.3 g (23% yield) of the title compound as pale yellow solids.

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. stirringThe mixture was stirred at 0° C. for 3 hours
  3. temperaturewarmed to room temperature
  4. customThe reaction was quenched with MeOH
  5. stirringstirred for 30 minutes
  6. additionThen to the mixuture water was added
  7. stirringAfter stirring for 10 minutes
  8. filtrationthe resulting suspension was filtered through a celite pad
  9. washthe filtered cake was washed with EtOAc
  10. concentrationThe filtrate was concentrated under reduced pressure
  11. customto give a residue, which
  12. washeluted with a volume mixture of DCM and EtOAc (1/1)

出典と根拠

ORDレコード
ord-4516348dd394486280fad9a47c69c668
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07622589B2

反応ノート

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