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4-Fluorobenzylamine → HCID 22346292, 화합물

HRID 897308
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HRID 897308 반응식
C([O:9][C:10]1[C:11]([C:27]([O:29]C)=O)=[N:12][C:13]([O:20][CH2:21][C:22]([N:24]([CH3:26])[CH3:25])=[O:23])=[C:14]2[C:19]=1[N:18]=[CH:17][CH:16]=[CH:15]2)(=O)C1C=CC=CC=1.[F:31][C:32]1[CH:39]=[CH:38][C:35]([CH2:36][NH2:37])=[CH:34][CH:33]=1>C1(C)C=CC=CC=1>[F:31][C:32]1[CH:39]=[CH:38][C:35]([CH2:36][NH:37][C:27]([C:11]2[C:10]([OH:9])=[C:19]3[C:14]([CH:15]=[CH:16][CH:17]=[N:18]3)=[C:13]([O:20][CH2:21][C:22]([N:24]([CH3:25])[CH3:26])=[O:23])[N:12]=2)=[O:29])=[CH:34][CH:33]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 673264-FluorobenzylamineHCID 22346259HCID 22346259, 화합물

생성물 1

HCID 22346292HCID 22346292, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
110 °C

실험 절차

A mixture of methyl ester from Step 1 (0.28 g, 0.68 mmol) and 4-fluorobenzylamine (0.16 mL, 1.43 mmol) in toluene (5 mL) was heated in an oil bath at 110° C. overnight. The resultant precipitate was filtered, washed with diethyl ether, and dried under vacuum. The solid was dissolved in DMSO and subjected to HPLC purification on C-18 stationary phase eluted with water/acetonitrile/TFA mobile phase. Collection and lyophilization of appropriate fractions provided the title compound as yellow solid.

후처리

  1. filtrationThe resultant precipitate was filtered
  2. washwashed with diethyl ether
  3. customdried under vacuum
  4. dissolutionThe solid was dissolved in DMSO
  5. customsubjected to HPLC purification on C-18 stationary phase
  6. washeluted with water/acetonitrile/TFA mobile phase
  7. customCollection and lyophilization of appropriate fractions

출처 및 근거

ORD 기록
ord-2a9fa19e028040bf8f24c0c3869e98c5
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06921759B2

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