4-Fluorobenzylamine → HCID 448749, 화합물

HRID 2219055노트

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HRID 2219055 반응식
[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH2:7])=[CH:4][CH:3]=1.[OH:10][C:11]1[C:30](=[O:31])[N:15]2[CH2:16][CH2:17][CH2:18][CH2:19][CH:20]([NH:21][C@@H:22]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH3:23])[C:14]2=[N:13][C:12]=1[C:32](OC)=[O:33]>CO>[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH:7][C:32]([C:12]2[N:13]=[C:14]3[CH:20]([NH:21][C@@H:22]([C:24]4[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=4)[CH3:23])[CH2:19][CH2:18][CH2:17][CH2:16][N:15]3[C:30](=[O:31])[C:11]=2[OH:10])=[O:33])=[CH:4][CH:3]=1.[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH3+:7])=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 673264-FluorobenzylamineHCID 67148233HCID 67148233, 화합물

생성물 2

HCID 448749HCID 448749, 화합물HCID 67148197HCID 67148197, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

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온도
70 °C

실험 절차

p-Fluorobenzylamine (3 eq.) was added to the methyl 3-hydroxy-4-oxo-10-{[(1R)-1-phenylethyl]amino}-4,6,7,8,9,10-hexahydropyrimido[1,2-a]azepine-2-carboxylate (prepared as described in Step 5 or Step 5A) dissolved in methanol. The mixture was stirred at 70° C. overnight, then cooled to room temperature for use directly in Step 7. In an alternative procedure (Step 6A), the solvent was removed and the crude product crystallized from acetonitrile several times to obtain a single diasteroisomer of the title compound as the 4-fluorobenzylammonium salt with d.e.>95%

후처리

  1. temperaturecooled to room temperature for use directly in Step 7
  2. customIn an alternative procedure (Step 6A), the solvent was removed
  3. customthe crude product crystallized from acetonitrile several times

출처 및 근거

ORD 기록
ord-46dda1c810c44ed189e84de56743609f
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07414045B2

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