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 528782노트

반응식

HRID 528782 반응식
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

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acid2회HCID 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

생성물 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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f698ac6e7dbb40a7a6b0d062b529fc36
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346816B2

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