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Water → HCID 117966289, 화합물

HRID 931101
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HRID 931101 반응식
[CH:1]1[N:5]=[C:4]([CH:6]2[CH2:11][CH2:10][CH2:9][N:8]([C:12]3[N:17]=[C:16]([NH2:18])[C:15]([N+:19]([O-])=O)=[CH:14][CH:13]=3)[CH2:7]2)[N:3]2[CH2:22][CH2:23][CH2:24][C:2]=12.O.[Cl-:26].[Ca+2].[Cl-]>C(O)C.[Fe]>[ClH:26].[CH:1]1[N:5]=[C:4]([CH:6]2[CH2:11][CH2:10][CH2:9][N:8]([C:12]3[N:17]=[C:16]([NH2:18])[C:15]([NH2:19])=[CH:14][CH:13]=3)[CH2:7]2)[N:3]2[CH2:22][CH2:23][CH2:24][C:2]=12
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 5284359Calcium ChlorideHCID 89853740HCID 89853740, 화합물

생성물 1

HCID 117966289HCID 117966289, 화합물

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

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온도
70 °C

실험 절차

6-(3-(6,7-Dihydro-5H-pyrrolo[1,2-c]imidazol-3-yl)piperidin-1-yl)-3-nitropyridin-2-amine (20 mg, 0.1 mmol) was dissolved in ethanol (0.5 mL) and water (0.1 mL) under nitrogen. Then iron 200 mesh (27 mg, 0.5 mmol) and calcium chloride (3.3 mg, 0.03 mmol) were added and the mixture was heated to 70° C. for 18 h. The reaction mixture was cooled to room temperature followed by filtration through a 0.2 μm nylon syringe filter and rinsing with ethanol (0.5 mL) to afford the title compound. The filtrate was carried on to the next step without further purification. MS (AP+) (M+H) 299.1; LCMS retention time: 0.44 minutes (Method L)

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationfollowed by filtration through a 0.2 μm nylon syringe
  3. filtrationfilter
  4. washrinsing with ethanol (0.5 mL)

출처 및 근거

ORD 기록
ord-f4e48f74565346fcabc86cb3188d1261
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296745B2

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