Trifluoroacetic acid → (4,4-Difluoro-perhydro-azepin-1-yl)-[1-(6,7,8,9-tetrahydro-5H-1,4,7,10a-tetraaza-cyclohept[f]inden-10-yl)-azetidin-3-yl]-methanone

HRID 528782ノート

反応式

HRID 528782 の反応式
C(OC([N:8]1[CH2:36][CH2:35][C:12]2=[C:13]([N:20]3[CH2:23][CH:22]([C:24]([N:26]4[CH2:32][CH2:31][CH2:30][C:29]([F:34])([F:33])[CH2:28][CH2:27]4)=[O:25])[CH2:21]3)[N:14]3[C:18]([N:19]=[C:11]2[CH2:10][CH2:9]1)=[CH:17][CH:16]=[N:15]3)=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[F:34][C:29]1([F:33])[CH2:30][CH2:31][CH2:32][N:26]([C:24]([CH:22]2[CH2:23][N:20]([C:13]3[N:14]4[C:18]([N:19]=[C:11]5[CH2:10][CH2:9][NH:8][CH2:36][CH2:35][C:12]=35)=[CH:17][CH:16]=[N:15]4)[CH2:21]2)=[O:25])[CH2:27][CH2:28]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acid2 回HCID 6797949110-[3-(4,4-Difluoro-perhydro-azepine-1-carbonyl)-azetidin-1-yl]-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohept[f]indene-7-carboxylic acid tert-butyl ester

生成物 1

HCID 46833161(4,4-Difluoro-perhydro-azepin-1-yl)-[1-(6,7,8,9-tetrahydro-5H-1,4,7,10a-tetraaza-cyclohept[f]inden-10-yl)-azetidin-3-yl]-methanone

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To 190 mg (0.38 mmol) 10-[3-(4,4-Difluoro-perhydro-azepine-1-carbonyl)-azetidin-1-yl]-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohept[f]indene-7-carboxylic acid tert-butyl ester in 5 mL DCM was added 0.38 mL TFA and stirring was continued overnight at room temperature. To neutralize TFA sat. NaHCO3-solution was added, the organic layer separated and dried over Na2SO4. After filtration and evaporation of the solvent was the residue purified by HPLC.

後処理

  1. additionwas added
  2. customthe organic layer separated
  3. dry with materialdried over Na2SO4
  4. filtrationAfter filtration and evaporation of the solvent
  5. custompurified by HPLC

出典と根拠

ORDレコード
ord-f698ac6e7dbb40a7a6b0d062b529fc36
出典データセット
uspto-grants-2016_05
特許番号
US09346816B2

反応ノート

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