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Hydrochloric Acid → HCID 66656409, 화합물

HRID 517780
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HRID 517780 반응식
[F:1][C:2]([F:30])([F:29])[C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:13]([CH2:14][N:15]3[CH2:20][C@@H:19]4[CH2:21][C@H:16]3[CH2:17][N:18]4C(OC(C)(C)C)=O)=[N:12][N:11]=[N:10]2)=[CH:5][CH:4]=1.Cl.O1CCOCC1>CO>[F:30][C:2]([F:1])([F:29])[C:3]1[CH:4]=[CH:5][C:6]([N:9]2[C:13]([CH2:14][N:15]3[CH2:20][C@@H:19]4[CH2:21][C@H:16]3[CH2:17][NH:18]4)=[N:12][N:11]=[N:10]2)=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 68297709HCID 68297709, 화합물2회

생성물 1

HCID 66656409HCID 66656409, 화합물수율 101.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 1,1-dimethylethyl (1S,4S)-5-({1-[4-(trifluoromethyl)phenyl]-1H-tetrazol-5-yl}methyl)-2,5-diazabicyclo[2.2.1]heptane-2-carboxylate (470 mg, 1.107 mmol, Intermediate 17) in methanol was added 4M hydrogen chloride in 1,4-dioxane (5 mL, 20 mmol). The reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was concentrated in vacuo and poured onto a 5 g SCX cartridge. The cartridge was washed with methanol (2 column volumes) and eluted with ammonia in methanol (2 column volumes). The ammonia in methanol fractions were concentrated and the residue dried in vacuo to yield the title compound as white crystals (363 mg)

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additionpoured onto a 5 g SCX cartridge
  3. washThe cartridge was washed with methanol (2 column volumes)
  4. washeluted with ammonia in methanol (2 column volumes)
  5. concentrationThe ammonia in methanol fractions were concentrated
  6. customthe residue dried in vacuo

출처 및 근거

ORD 기록
ord-28bc916c733b40638d6d199f28b8680d
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115132B2

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