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Hydrochloric Acid → HCID 67610940, 화합물

HRID 1418391
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HRID 1418391 반응식
C1O[C:4]2([CH2:9][CH2:8][N:7]([C:10]([N:12]3[CH:16]=[CH:15][N:14]=[CH:13]3)=[O:11])[CH2:6][CH2:5]2)OC1.[ClH:18].Cl.[NH2:20][C:21]1[CH:29]=[CH:28][CH:27]=[C:26]([F:30])[C:22]=1[C:23]([NH2:25])=[NH:24].Cl>C(O)C>[ClH:18].[NH2:25][C:23]1[C:22]2[C:21](=[CH:29][CH:28]=[CH:27][C:26]=2[F:30])[NH:20][C:4]2([CH2:5][CH2:6][N:7]([C:10]([N:12]3[CH:16]=[CH:15][N:14]=[CH:13]3)=[O:11])[CH2:8][CH2:9]2)[N:24]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 12185909HCID 12185909, 화합물HCID 22008823HCID 22008823, 화합물

생성물 1

HCID 67610940HCID 67610940, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
55 °C

실험 절차

1-(1H-Imidazol-1-ylcarbonyl)-4-piperidone ethylene ketal (Example EE, 156 mg., 0.66 mmol) was added to 2-amino-6-fluorobenzamidine dihydrochloride (150 mg, 0.66 is mmol) in ethanol (10 ml) together with an excess of HCl (1M in ether). This mixture was heated to 55° C. overnight, concentrated in vacuo and purified by flash column chromatography eluting with dichloromethane, increasing the gradient to dichloromethane/methanol (10:1), to give a solid which triturated from ethanol/ether to give yellow crystals, m.p. 260° C. (dec.).

후처리

  1. concentrationconcentrated in vacuo
  2. custompurified by flash column chromatography
  3. washeluting with dichloromethane
  4. temperatureincreasing the gradient to dichloromethane/methanol (10:1)
  5. customto give a solid which
  6. customtriturated from ethanol/ether
  7. customto give yellow crystals, m.p. 260° C. (dec.)

출처 및 근거

ORD 기록
ord-e458bfbb3c15431aa15886bf6867d3ee
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05883102

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