HCID 68828337、化合物 → HCID 11570771、化合物

HRID 2099352ノート

反応式

HRID 2099352 の反応式
[Cl:1][C:2]1[CH:47]=[CH:46][C:5]([CH2:6][C@@H:7]([NH:32][CH:33]2[CH2:38][CH2:37][N:36](C(OC(C)(C)C)=O)[CH2:35][CH2:34]2)[C:8]([N:10]2[CH:15]3[CH2:16][CH2:17][CH:11]2[CH2:12][CH:13]([N:18]([CH:26]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]2)[C:19]([N:21]([CH2:24][CH3:25])[CH2:22][CH3:23])=[O:20])[CH2:14]3)=[O:9])=[CH:4][CH:3]=1>Cl.C(OCC)C>[ClH:1].[Cl:1][C:2]1[CH:47]=[CH:46][C:5]([CH2:6][C@H:7]([C:8]([N:10]2[CH:15]3[CH2:16][CH2:17][CH:11]2[CH2:12][CH:13]([N:18]([CH:26]2[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]2)[C:19]([N:21]([CH2:22][CH3:23])[CH2:24][CH3:25])=[O:20])[CH2:14]3)=[O:9])[NH:32][CH:33]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]2)=[CH:4][CH:3]=1

参加物

4

反応物 1

HCID 68828337HCID 68828337、化合物

生成物 1

HCID 11570771HCID 11570771、化合物収率 161.2%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 3283Diethyl Ether溶媒

実験手順

0.37 g of tert-butyl 4-{[(1R)-1-(4-chlorobenzyl)-2-(3-{cyclohexyl[(diethylamino)carbonyl]amino}-8-azabicyclo[3.2.1]oct-8-yl)-2-oxoethyl]amino}-piperidine-1-carboxylate is solubilized in 2.74 ml of 2N hydrochloric acid in diethyl ether. The reaction medium is stirred at ambient temperature for 16 h. After evaporation to dryness, the crude is chromatographed on silica gel, elution being carried out with a 95/5/0.5 mixture of dichloromethane, methanol and aqueous ammonia. 0.27 g of N-[8-(4-chloro-N-piperidin-4-yl-D-phenylalanyl)-8-azabicyclo-[3.2.1]oct-3-yl]-N-cyclohexyl-N′,N′-diethylurea hydrochloride is then obtained.

後処理

  1. customAfter evaporation to dryness
  2. customthe crude is chromatographed on silica gel, elution
  3. additionbeing carried out with a 95/5/0.5 mixture of dichloromethane, methanol and aqueous ammonia

出典と根拠

ORDレコード
ord-8ea7520a4b1e4b03afd66ce1733249df
出典データセット
uspto-grants-2009_08
特許番号
US07569582B2

反応ノート

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