4-Fluorobenzylamine → HCID 448749、化合物

HRID 2426268ノート

反応式

HRID 2426268 の反応式
[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

参加物

5

反応物 2

HCID 673264-FluorobenzylamineHCID 67148233HCID 67148233、化合物

生成物 2

HCID 448749HCID 448749、化合物HCID 67148197HCID 67148197、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

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 diastereoisomer of the title compound as the 4-fluorobenzylammonium salt with d.e.>95%

後処理

  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

出典と根拠

ORDレコード
ord-db0f0a347e26408f89a81faed7481ae6
出典データセット
uspto-grants-2011_06
特許番号
US07968553B2

反応ノート

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