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Methanesulfonic acid, trifluoro-, 2-methyl-3-oxo-1-cyclohexen-1-yl ester → (10,11-Dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-10-yl)-[2-chloro-4-(2-methyl-3-oxo-cyclohex-1-en-1-yl)-phenyl]-methanone

HRID 1793982
ノート
印刷プレビュー

反応式

HRID 1793982 の反応式
[CH:1]1[CH:2]=[CH:3][N:4]2[CH2:10][C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[N:7]([C:15]([C:17]3[CH:22]=[CH:21][C:20](B4OC(C)(C)C(C)(C)O4)=[CH:19][C:18]=3[Cl:32])=[O:16])[CH2:6][C:5]=12.FC(F)(F)S([O:38][C:39]1[CH2:44][CH2:43][CH2:42][C:41](=O)[C:40]=1[CH3:46])(=O)=O>C(OCC)C>[CH:1]1[CH:2]=[CH:3][N:4]2[CH2:10][C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[N:7]([C:15]([C:17]3[CH:22]=[CH:21][C:20]([C:41]4[CH2:42][CH2:43][CH2:44][C:39](=[O:38])[C:40]=4[CH3:46])=[CH:19][C:18]=3[Cl:32])=[O:16])[CH2:6][C:5]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 10825071Methanesulfonic acid, trifluoro-, 2-methyl-3-oxo-1-cyclohexen-1-yl esterHCID 22219716(10,11-Dihydro-5H-pyrrolo[2,1-c](1,4]benzodiazepin-10-yl)-[2-chloro-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-methanone

生成物 1

HCID 10203009(10,11-Dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-10-yl)-[2-chloro-4-(2-methyl-3-oxo-cyclohex-1-en-1-yl)-phenyl]-methanone収率 53.6%

試薬・触媒・溶媒 1

HCID 3283
Diethyl Ether
溶媒

実験手順

(10,11-Dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-10-yl)-[2-chloro-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-methanone of Example 10, Step B (0.350 g, 0.780 mmol) and 2-methyl-3-oxo-cyclohex-1-en-1-yl trifluoromethanesulfonate (0.222 g, 0.858 mmol) were reacted by the procedure described in Example 1, Step F. The crude product was purified by flash column chromatography on silica gel, eluting with 50% ethyl acetate in hexane to afford an orange oil. The oil was dissolved in diethyl ether and precipitated with petroleum ether to afford orange solid (0.180 g).

後処理

  1. customThe crude product was purified by flash column chromatography on silica gel
  2. washeluting with 50% ethyl acetate in hexane
  3. customto afford an orange oil
  4. customprecipitated with petroleum ether

出典と根拠

ORDレコード
ord-18e53be3219a453381dcea39c67c502c
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07022699B2

反応ノート

読み込み中…

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