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Dimethylformamide → (6R)-6-(5-chloro-2-methoxybenzyl)-N-[(1R)-1-(3-tert-butoxyisooxazole-5-yl)propyl]-3,7-dioxo-4-(2,4,6-trimethoxybenzyl)-1,4-diazepane-1-carboxamide

HRID 80585
ノート
印刷プレビュー

反応式

HRID 80585 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:41][CH3:42])=[C:6]([CH:40]=1)[CH2:7][C@H:8]1[C:14](=[O:15])[N:13]([C:16](OC2C=CC=CC=2Cl)=[O:17])[CH2:12][C:11](=[O:26])[N:10]([CH2:27][C:28]2[C:33]([O:34][CH3:35])=[CH:32][C:31]([O:36][CH3:37])=[CH:30][C:29]=2[O:38][CH3:39])[CH2:9]1.CN(C)C=O.Cl.[C:49]([O:53][C:54]1[CH:58]=[C:57]([CH:59]([NH2:62])[CH2:60][CH3:61])[O:56][N:55]=1)([CH3:52])([CH3:51])[CH3:50].C(N(CC)C(C)C)(C)C>CN(C)C1C=CN=CC=1.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:41][CH3:42])=[C:6]([CH:40]=1)[CH2:7][C@H:8]1[C:14](=[O:15])[N:13]([C:16]([NH:62][C@@H:59]([C:57]2[O:56][N:55]=[C:54]([O:53][C:49]([CH3:50])([CH3:52])[CH3:51])[CH:58]=2)[CH2:60][CH3:61])=[O:17])[CH2:12][C:11](=[O:26])[N:10]([CH2:27][C:28]2[C:29]([O:38][CH3:39])=[CH:30][C:31]([O:36][CH3:37])=[CH:32][C:33]=2[O:34][CH3:35])[CH2:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 81531DiisopropylethylamineHCID 66935304(6R)-2-chlorophenyl 6-(5-chloro-2-methoxybenzyl)-3,7-dioxo-4-(2,4,6-trimethoxybenzyl)-1,4-diazepan-1-carboxylateHCID 708152761-(3-Tert-butoxyisoxazol-5-yl)propylamine hydrochloride

生成物 1

HCID 70815060
(6R)-6-(5-chloro-2-methoxybenzyl)-N-[(1R)-1-(3-tert-butoxyisooxazole-5-yl)propyl]-3,7-dioxo-4-(2,4,6-trimethoxybenzyl)-1,4-diazepane-1-carboxamide
収率 43%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 962Water溶媒

実験手順

To the compound S141C described in WO 06-059801A, that is, (6R)-2-chlorophenyl 6-(5-chloro-2-methoxybenzyl)-3,7-dioxo-4-(2,4,6-trimethoxybenzyl)-1,4-diazepane-1-carboxylate (395 mg) in an N,N-dimethylformamide (0.64 ml) solution, the compound S94 described in WO 06-059801A, that is, 1-(3-tert-butoxyisoxazol-5-yl)propylamine hydrochloride (150 mg), 4-dimethylaminopyridin (78 mg) and N,N-diisopropylethylamine (0.111 ml) were added at 0° C., and the mixture was stirred at that temperature for 15 hours. To the reaction solution, water was added, and the mixture was extracted with ethyl acetate. The extract was combined, successively washed with saturated aqueous potassium hydrogensulfate solution, saturated aqueous sodium hydrogencarbonate solution, and brine, dried over sodium sulfate, then concentrated. The residue was purified by flash column chromatography (silica gel, hexane/ethyl acetate=50/50 to 35/65) to obtain (6R)-6-(5-chloro-2-methoxybenzyl)-N-[(1R)-1-(3-tert-butoxyisooxazole-5-yl)propyl]-3,7-dioxo-4-(2,4,6-trimethoxybenzyl)-1,4-diazepane-1-carboxamide (189 mg) (compound S49a) and (6R)-6-(5-chloro-2-methoxybenzyl)-N-[(1S)-1-(3-tert-butoxyisooxazol-5-yl)propyl]-3,7-dioxo-4-(2,4,6-trimethoxybenzyl)-1,4-diazepane-1-carboxamide (compound S49b).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washsuccessively washed with saturated aqueous potassium hydrogensulfate solution, saturated aqueous sodium hydrogencarbonate solution, and brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by flash column chromatography (silica gel, hexane/ethyl acetate=50/50 to 35/65)

出典と根拠

ORDレコード
ord-89be20f1e1df46f7becb2bedadd688c9
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846660B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート