N-((1,1-dimethylethoxy)carbonyl)-beta-alanine → N-(9-chloro-3,4-dihydro-2H-1,5-benzodioxepin-7-ylmethyl)-N-isobutyl 3-[(2-methylpropan-2-yl)oxycarbonylamino]propanamide

HRID 1024496

反応式

HRID 1024496 の反応式
[Cl:1][C:2]1[C:7]2[O:8][CH2:9][CH2:10][CH2:11][O:12][C:6]=2[CH:5]=[C:4]([CH2:13][NH:14][CH2:15][CH:16]([CH3:18])[CH3:17])[CH:3]=1.[CH3:19][C:20]([O:23][C:24]([NH:26][CH2:27][CH2:28][C:29](O)=[O:30])=[O:25])([CH3:22])[CH3:21].Cl.C(N=C=NCCCN(C)C)C.CC1C=CN=C(N)C=1C>ClCCl>[Cl:1][C:2]1[C:7]2[O:8][CH2:9][CH2:10][CH2:11][O:12][C:6]=2[CH:5]=[C:4]([CH2:13][N:14]([CH2:15][CH:16]([CH3:18])[CH3:17])[C:29](=[O:30])[CH2:28][CH2:27][NH:26][C:24]([O:23][C:20]([CH3:21])([CH3:19])[CH3:22])=[O:25])[CH:3]=1

参加物

6

反応物 4

HCID 76809N-((1,1-dimethylethoxy)carbonyl)-beta-alanineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 110078842-Amino-3,4-dimethylpyridineHCID 43087680N-(9-chloro-3,4-dihydro-2H-1,5-benzodioxepin-7-ylmethyl)-2-methylpropan-1-amine

生成物 1

HCID 66726199N-(9-chloro-3,4-dihydro-2H-1,5-benzodioxepin-7-ylmethyl)-N-isobutyl 3-[(2-methylpropan-2-yl)oxycarbonylamino]propanamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of N-(9-chloro-3,4-dihydro-2H-1,5-benzodioxepin-7-ylmethyl)-2-methylpropan-1-amine (140 mg), 3-[(2-methylpropan-2-yl)oxycarbonylamino]propanoic acid (Boc-beta-alanine, 98 mg), of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (163 mg), and of dimethyl aminopyridine (113 mg) in dichloromethane (10 ml) was stirred overnight. The mixture was concentrated under reduced pressure. Desired compound [N-(9-chloro-3,4-dihydro-2H-1,5-benzodioxepin-7-ylmethyl)-N-isobutyl 3-[(2-methylpropan-2-yl)oxycarbonylamino]propanamide] was isolated by flash chromatography on silica (100% dichloromethane) as a resin: MS (m+1)=441.3.

後処理

  1. concentrationThe mixture was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-da5d9a6fd3474bba85745d31150650f1
出典データセット
uspto-grants-2014_05
特許番号
US08722896B2

関連ノート

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