Acetate-hydrochloric acid → HCID 11634767、化合物

HRID 554773ノート

反応式

HRID 554773 の反応式
[NH2:1][C:2]1[CH:14]=[C:13]([C@H:15]([NH:18][C:19]([N:21]2[C:27](=[O:28])[C@@H:26]([CH2:29][C:30]3[CH:35]=[C:34]([Cl:36])[CH:33]=[CH:32][C:31]=3[O:37][CH3:38])[CH2:25][N:24](CC3C(OC)=CC(OC)=CC=3OC)[C:23](=[O:52])[CH2:22]2)=[O:20])[CH2:16][CH3:17])[CH:12]=[CH:11][C:3]=1[C:4]([O:6]C(C)(C)C)=[O:5].Cl.C(O)(=O)C>>[NH2:1][C:2]1[CH:14]=[C:13]([C@H:15]([NH:18][C:19]([N:21]2[C:27](=[O:28])[C@@H:26]([CH2:29][C:30]3[CH:35]=[C:34]([Cl:36])[CH:33]=[CH:32][C:31]=3[O:37][CH3:38])[CH2:25][NH:24][C:23](=[O:52])[CH2:22]2)=[O:20])[CH2:16][CH3:17])[CH:12]=[CH:11][C:3]=1[C:4]([OH:6])=[O:5]

参加物

3

反応物 2

HCID 22641269Acetate-hydrochloric acidHCID 66934849HCID 66934849、化合物

生成物 1

HCID 11634767HCID 11634767、化合物収率 28%

実験手順

(Step 2) To tert-butyl 2-amino-4-[(1R)-1-({[(6S)-6-(5-chloro-2-methoxybenzyl)-3,7-dioxo-4-(2,4,6-trimethoxybenzyl)-1,4-diazepan-1-yl]carbonyl}amino)propyl]benzoate (1.47 g), 1M hydrogen chloride/acetic acid solution (15 ml) was added and the mixture was stirred at room temperature for 20 hours. The reaction solution was concentrated, then the residue was purified by silica gel column chromatography (chloroform/ethyl acetate/methanol/acetic acid=8/8/1/0.1) to obtain the title compound (0.28 g).

後処理

  1. concentrationThe reaction solution was concentrated
  2. customthe residue was purified by silica gel column chromatography (chloroform/ethyl acetate/methanol/acetic acid=8/8/1/0.1)

出典と根拠

ORDレコード
ord-3bc9d176b6774663b188635823d29330
出典データセット
uspto-grants-2011_11
特許番号
US08049006B2

反応ノート

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