Phosphoric Acid → HCID 21091439、化合物

HRID 1348601ノート

反応式

HRID 1348601 の反応式
C(OC(=O)[NH:7][C@@H:8]1[C:14](=[O:15])[N:13]([CH2:16][C:17]([F:20])([F:19])[F:18])[C:12]2[CH:21]=[C:22]([F:25])[CH:23]=[CH:24][C:11]=2[O:10][C@@H:9]1[CH3:26])(C)(C)C.P(=O)(O)(O)O>O1CCCC1>[NH2:7][C@@H:8]1[C:14](=[O:15])[N:13]([CH2:16][C:17]([F:18])([F:20])[F:19])[C:12]2[CH:21]=[C:22]([F:25])[CH:23]=[CH:24][C:11]=2[O:10][C@@H:9]1[CH3:26]

参加物

4

反応物 2

HCID 1004Phosphoric AcidHCID 67077130[(6R,7S)-2-fluoro-6-methyl-8-oxo-9-(2,2,2-trifluoro-ethyl)-6,7,8,9-tetrahydro-5-oxa-9-aza-benzocyclohepten-7-yl]-carbamic acid tert-butyl ester

生成物 1

HCID 21091439HCID 21091439、化合物収率 83.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 0.50 g (1.27 mmol) [(6R,7S)-2-fluoro-6-methyl-8-oxo-9-(2,2,2-trifluoro-ethyl)-6,7,8,9-tetrahydro-5-oxa-9-aza-benzocyclohepten-7-yl]-carbamic acid tert-butyl ester in 5 ml tetrahydrofurane were added 1.89 g ortho-phosphoric acid. The mixture was stirred at room temperature for 2 days. Extraction with ethylacetate/water and chromatography on silicagel with dichloromethane/methanol 98/2 yielded 0.31 g (83%) (6R,7S)-7-amino-2-fluoro-6-methyl-9-(2,2,2-trifluoro-ethyl)-6,7-dihydro-9H-5-oxa-9-aza-benzocyclohepten-8-one, MS m/e (%): 293.1 (M+H+, 100).

後処理

  1. extractionExtraction with ethylacetate/water and chromatography on silicagel with dichloromethane/methanol 98/2

出典と根拠

ORDレコード
ord-2c7fe17cbbf044dd8c8a9f1e2acf6cb4
出典データセット
uspto-grants-2007_05
特許番号
US07211573B2

反応ノート

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