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Dichloromethane → Azepan-1-yl-(5-pyridin-4-yl-thiophen-3-yl)-methanone

HRID 1914554
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인쇄 미리보기

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HRID 1914554 반응식
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[S:11][CH:10]=[C:9]([C:12]([OH:14])=O)[CH:8]=2)=[CH:3][CH:2]=1.[N:15]1([C:22](=O)[CH3:23])[CH2:21][CH2:20][CH2:19]NCC1.[CH3:25]N(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(Cl)Cl>CC#N>[N:15]1([C:12]([C:9]2[CH:8]=[C:7]([C:4]3[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=3)[S:11][CH:10]=2)=[O:14])[CH2:21][CH2:20][CH2:19][CH2:25][CH2:23][CH2:22]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 4186202N-AcetylhomopiperazineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 581102285-Pyridin-4-yl-thiophene-3-carboxylic acid

생성물 1

HCID 44224462Azepan-1-yl-(5-pyridin-4-yl-thiophen-3-yl)-methanone수율 28.8%

시약·촉매·용매

1
HCID 6342Acetonitrile용매

실험 절차

5-Pyridin-4-yl-thiophene-3-carboxylic acid (0.4 mmol) was dissolved in MeCN (2 mL). 1-[1,4]Diazepan-1-yl-ethanone (1.8 mmol), and HATU (0.4 mmol) were added and the reaction mixture stirred for 72 hours. DCM (20 mL) was added and the organic solution was separated and the solvent removed by evaporation. The residue was purified by HPLC, eluting with 10%-90% acetonitrile in water (0.1% formic acid) over 30 minutes. The fractions containing the desired product were concentrated under vacuum and freeze-dried to give the title compound as a white solid (33 mg). LCMS m/z 287.09 [M+H]+ RT=5.20 min. (Analytical Method 2). 1H NMR (400 MHz, MeCN-d): δ 8.6 (d, 2H), 7.95 (d, 2H), 7.9 (s, 1H), 7.8 (s, 1H), 3.6 (t, 2H), 3.5 (t, 2H), 1.8-1.6 (m, 6H).

후처리

  1. customthe organic solution was separated
  2. customthe solvent removed by evaporation
  3. customThe residue was purified by HPLC
  4. washeluting with 10%-90% acetonitrile in water (0.1% formic acid) over 30 minutes
  5. additionThe fractions containing the desired product
  6. concentrationwere concentrated under vacuum
  7. customfreeze-dried

출처 및 근거

ORD 기록
ord-72e456684d454ab8ab41a2981dbf7f33
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08614209B2

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