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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethyl 2-bromopropionate → Piperidin-1-yl-acetic acid

HRID 1989878
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인쇄 미리보기

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HRID 1989878 반응식
BrC(C)C(OCC)=O.Cl.C1([CH:16]([N:20]2[CH2:25][CH2:24][CH:23](C3C=CC(NC(C4C=CC=CC=4C4C=CC(C(F)(F)F)=CC=4)=O)=CC=3)[CH2:22][CH2:21]2)[C:17]([OH:19])=[O:18])C=CC=CC=1.C(NC(=S)N(CCCC)CCCC)CCC>CCN(C(C)C)C(C)C>[N:20]1([CH2:16][C:17]([OH:19])=[O:18])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 79040Ethyl 2-bromopropionateHCID 3032425TributylthioureaHCID 67460709HCID 67460709, 화합물

생성물 1

HCID 201097Piperidin-1-yl-acetic acid

시약·촉매·용매 1

HCID 81531Diisopropylethylamine용매

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온도
70 °C

실험 절차

Ethyl 2-bromopropionate (0.0001 mol) was added to a mixture of intermediate (12) (0.000084 mol) and tri-n-butylthiourea (TBTU) (0.000168 mol) in DIPEA (4 ml). The reaction mixture was shaken for 2 hours at 70° C. The reaction mixture was cooled to room temperature, filtered and the filtrate was evaporated. The residue was dissolved in DCM (4 ml), then washed with water (2 ml). The mixture was filtered through Extrelut™ and the filter residue was washed with DCM (2×3 ml). The filtrate was evaporated. The residue was purified by HPLC (Waters column, with Xterra MS C18; eluent: [(0.5% NH4OAc in H2O)/CH3CN 90/10)]/CH3CN (0 min) 85/15, (10 min) 10/90, (16 min) 0/100, (18.10-20.00 min) 85/15), yielding 1-piperidineacetic acid, α-phenyl-4-[4-[[[4′-(trifluoromethyl)[1,1′-biphenyl]-2-yl]carbonyl]amino]phenyl]-, 2-ethoxy-1-methyl-2-oxoethyl ester (compound 111).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationfiltered
  3. customthe filtrate was evaporated
  4. dissolutionThe residue was dissolved in DCM (4 ml)
  5. washwashed with water (2 ml)
  6. filtrationThe mixture was filtered through Extrelut™
  7. washthe filter residue was washed with DCM (2×3 ml)
  8. customThe filtrate was evaporated
  9. customThe residue was purified by HPLC (Waters column

출처 및 근거

ORD 기록
ord-44f300cc2e9f47e988b009f58ede8876
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07642378B2

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