3,5-Difluorophenylacetic acid → 3[N'-(3,5-Difluorophenylacetyl)-L-alaninyl]amino-2,4-dioxo-1,5bis-(2-methylpropyl)-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine

HRID 1264748

反応式

HRID 1264748 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]([OH:12])=O)[CH:5]=[C:6]([F:8])[CH:7]=1.Cl.[NH2:14][C@H:15]([C:17]([NH:19][CH:20]1[C:26](=[O:27])[N:25]([CH2:28][CH:29]([CH3:31])[CH3:30])[C:24]2[CH:32]=[CH:33][CH:34]=[CH:35][C:23]=2[N:22]([CH2:36][CH:37]([CH3:39])[CH3:38])[C:21]1=[O:40])=[O:18])[CH3:16]>>[F:8][C:6]1[CH:5]=[C:4]([CH2:9][C:10]([NH:14][C@H:15]([C:17]([NH:19][CH:20]2[C:21](=[O:40])[N:22]([CH2:36][CH:37]([CH3:38])[CH3:39])[C:23]3[CH:35]=[CH:34][CH:33]=[CH:32][C:24]=3[N:25]([CH2:28][CH:29]([CH3:31])[CH3:30])[C:26]2=[O:27])=[O:18])[CH3:16])=[O:12])[CH:3]=[C:2]([F:1])[CH:7]=1

参加物

3

反応物 2

HCID 1454243,5-Difluorophenylacetic acidHCID 235527663-(L-alaninyl)amino-2,4-dioxo-1,5-bis-(2-methylpropyl)-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine hydrochloride

生成物 1

HCID 229840813[N'-(3,5-Difluorophenylacetyl)-L-alaninyl]amino-2,4-dioxo-1,5bis-(2-methylpropyl)-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine

実験手順

Following General Procedure I above using 3,5-difluorophenylacetic acid (Lancaster) and 3-(L-alaninyl)amino-2,4-dioxo-1,5-bis-(2-methylpropyl)-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine hydrochloride (Example 8-S), the title compound was prepared as a white solid (melting point=197-198° C.). Purification was by flash chromatography eluting with CH2Cl2/EtOAc (2:1 gradient to 3:4). Rf=0.23 (CH2Cl2/EtOAc, 1:1).

後処理

  1. customPurification
  2. washeluting with CH2Cl2/EtOAc (2:1 gradient to 3:4)

出典と根拠

ORDレコード
ord-92e5f275c22d4ca9af134e7d65b260dc
出典データセット
uspto-grants-2003_04
特許番号
US06544978B2

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