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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Trifluoroacetic acid → HCID 86726690, 화합물

HRID 1499446
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HRID 1499446 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[S:10][CH:11]=[C:12]([C:14]([NH:16][C:17]2[C:18]([N:26]3[CH2:31][CH2:30][CH2:29][C@H:28]([NH:32]C(=O)OC(C)(C)C)[CH2:27]3)=[C:19]3[CH2:25][CH2:24][CH2:23][C:20]3=[N:21][CH:22]=2)=[O:15])[N:13]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl.CO.[NH4+].[OH-]>[NH2:32][C@H:28]1[CH2:29][CH2:30][CH2:31][N:26]([C:18]2[C:17]([NH:16][C:14]([C:12]3[N:13]=[C:9]([C:3]4[C:4]([F:8])=[CH:5][CH:6]=[CH:7][C:2]=4[F:1])[S:10][CH:11]=3)=[O:15])=[CH:22][N:21]=[C:20]3[CH2:23][CH2:24][CH2:25][C:19]=23)[CH2:27]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 6422Trifluoroacetic acidHCID 86726689HCID 86726689, 화합물

생성물 1

HCID 86726690HCID 86726690, 화합물수율 59.6%

시약·촉매·용매 3

HCID 887Methanol용매HCID 6344Dichloromethane용매HCID 14923Ammonium Hydroxide용매

실험 절차

tert-Butyl {(3S)-1-[3-({[2-(2,6-difluorophenyl)-1,3-thiazol-4-yl]carbonyl}amino)-6,7-dihydro-5H-cyclopenta[b]pyridin-4-yl]piperidin-3-yl}carbamate (4 mg, 0.007 mmol) was dissolved in DCM (0.02 mL) and then TFA (0.03 mL, 0.4 mmol) was added. The resulting reaction mixture was stirred at room temperature for 30 min. and then concentrated to give a residue, which was diluted with MeOH and neutralized with small amount of NH4OH. The mixture was filtered and purified by preparative LC-MS (XBridge™ preparative C18 30×10 mm, 5 m OBD™ column, at flow rate of 60 mL/min., eluting with a gradient of MeCN and water with 0.15% NH4OH) to afford the title compound (1.9 mg, 58%). LCMS calc. for C23H24F2N5OS (M+H)+: m/z=456.2. Found: 456.1.

후처리

  1. customThe resulting reaction mixture
  2. concentrationconcentrated
  3. customto give a residue, which
  4. filtrationThe mixture was filtered
  5. custompurified by preparative LC-MS (XBridge™ preparative C18 30×10 mm, 5 m OBD™ column
  6. washat flow rate of 60 mL/min., eluting with a gradient of MeCN and water with 0.15% NH4OH)

출처 및 근거

ORD 기록
ord-229bf454784f460c8f244a2446aeebfe
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09200004B2

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