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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → Tert-butyl(s)-1-((3ar,4s,6as)-4-(2,2-bis(4-fluorophenyl)acetamido)hexahydrocyclopenta[c]pyrrol-2(1h)-yl)-4-methyl-1-oxopentan-2-yl(methyl)carbamate

HRID 1092634
ノート
印刷プレビュー

反応式

HRID 1092634 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:20]2[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=2)[C:9]([NH:11][C@@H:12]2[C@@H:19]3[C@@H:15]([CH2:16][NH:17][CH2:18]3)[CH2:14][CH2:13]2)=[O:10])=[CH:4][CH:3]=1.[C:27]([O:31][C:32]([N:34]([CH3:43])[C@@H:35]([CH2:39][CH:40]([CH3:42])[CH3:41])[C:36](O)=[O:37])=[O:33])([CH3:30])([CH3:29])[CH3:28].O.ON1C2C=CC=CC=2N=N1.C(N=C=NCCCN(C)C)C>ClCCl>[F:26][C:23]1[CH:22]=[CH:21][C:20]([CH:8]([C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)[C:9]([NH:11][C@@H:12]2[C@@H:19]3[C@@H:15]([CH2:16][N:17]([C:36](=[O:37])[C@@H:35]([N:34]([CH3:43])[C:32](=[O:33])[O:31][C:27]([CH3:29])([CH3:28])[CH3:30])[CH2:39][CH:40]([CH3:42])[CH3:41])[CH2:18]3)[CH2:14][CH2:13]2)=[O:10])=[CH:25][CH:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 27960291-Hydroxybenzotriazole hydrateHCID 7010555(2S)-2-{[(tert-butoxy)carbonyl](methyl)amino}-4-methylpentanoic acidHCID 665911952,2-bis(4-fluorophenyl)-N-[(3aR,4S,6aS)-octahydrocyclopenta[c]pyrrol-4-yl]acetamide

生成物 1

HCID 66590861
Tert-butyl(s)-1-((3ar,4s,6as)-4-(2,2-bis(4-fluorophenyl)acetamido)hexahydrocyclopenta[c]pyrrol-2(1h)-yl)-4-methyl-1-oxopentan-2-yl(methyl)carbamate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2,2-Bis(4-fluorophenyl)-N-[(3aR,4S,6aS)-octahydrocyclopenta[c]pyrrol-4-yl]acetamide (30 mg, 0.084 mmol) and (S)-2-(tert-butoxycarbonyl(methyl)amino)-4-methylpentanoic acid (22.71 mg, 0.093 mmol) were dissolved in dichloromethane (0.5 mL) and then treated with 1-hydroxybenzotriazole hydrate (14.18 mg, 0.093 mmol). After 10 minutes, N1-((ethylimino)methylene)-N3,N3-dimethylpropane-1,3-diamine (0.016 mL, 0.093 mmol) was added, and the reaction mixture was stirred at ambient temperature overnight followed by quenching with water. The material in the organic layer was purified with a 4 g silica gel cartridge eluting with 1-10% methanol (2 N ammonia)/dichloromethane to give tert-butyl(S)-1-((3aR,4S,6aS)-4-(2,2-bis(4-fluorophenyl)acetamido)hexahydrocyclopenta[c]pyrrol-2(1H)-yl)-4-methyl-1-oxopentan-2-yl(methyl)carbamate: 1H NMR (400 MHz, pyridine-d5) δ ppm 8.25 (s, 1H), 7.46 (td, J=8.5, 5.5, 4H), 7.08-6.96 (m, 4H), 5.08 (s, 2H), 4.29-4.18 (m, 1H), 3.80 (s, 2H), 3.69 (s, 1H), 3.43 (dd, J=11.7, 3.5, 1H), 2.93 (s, 3H), 2.63 (s, 2H), 2.10 (td, J=12.9, 6.9, 1H), 1.91-1.69 (m, 3H), 1.63 (dt, J=13.2, 6.5, 2H), 1.51 (s, 9H), 1.40-1.26 (m, 1H), 0.97 (d, J=6.5, 3H), 0.92 (d, J=6.6, 3H); MS (ESI+) m/z 584 (M+H)+.

後処理

  1. customby quenching with water
  2. customThe material in the organic layer was purified with a 4 g silica gel cartridge
  3. washeluting with 1-10% methanol (2 N ammonia)/dichloromethane

出典と根拠

ORDレコード
ord-eeaea3113b7f4210ac0b5721af5be87c
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08129417B2

反応ノート

読み込み中…

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