ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1,2-Dichloroethane → 4-methyl-D-leucyl-N-[5-chloro-2-(1H-tetraazol-1-yl)benzyl]-L-prolinamide

HRID 857748
ノート
印刷プレビュー

反応式

HRID 857748 の反応式
[NH2:1][C@H:2]([C:7]([OH:9])=O)[CH2:3][CH:4]([CH3:6])[CH3:5].[Cl:10][C:11]1[CH:12]=[CH:13][C:14]([N:26]2[CH:30]=[N:29][N:28]=[N:27]2)=[C:15]([CH:25]=1)[CH2:16][NH:17][C:18](=[O:24])[C@@H:19]1[CH2:23][CH2:22][CH2:21][NH:20]1.[CH2:31](Cl)CCl.C1C=NC2N(O)N=NC=2C=1>CN(C=O)C.C(O)(C(F)(F)F)=O.C(Cl)Cl>[CH3:31][C:4]([CH3:5])([CH3:6])[CH2:3][C@H:2]([C:7]([N:20]1[CH2:21][CH2:22][CH2:23][C@H:19]1[C:18]([NH:17][CH2:16][C:15]1[CH:25]=[C:11]([Cl:10])[CH:12]=[CH:13][C:14]=1[N:26]1[CH:30]=[N:29][N:28]=[N:27]1)=[O:24])=[O:9])[NH2:1]
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 111,2-DichloroethaneHCID 6106L-LeucineHCID 181649HOAtHCID 69655818N-[5-chloro-2-(1H-tetraazol-1-yl)benzyl]-L-prolinamide

生成物 1

HCID 587601644-methyl-D-leucyl-N-[5-chloro-2-(1H-tetraazol-1-yl)benzyl]-L-prolinamide

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 21863450Trifluoroacetic acid methylene chloride溶媒

実験手順

The title compound was prepared from N-(tert-butoxycarbonyl)-4-methyl]-D-leucine (32 mg, 0.13 mmol), N-[5-chloro-2-(1H-1,2,4-tetraazol-1-yl)benzyl]-L-prolinamide (Example 26, Step B, 50 mg, 0.21 mmol, 1.0 equiv), EDC (38 mg, 0.20 mmol, 1.5 equiv) and HOAt (9 mg, 0.07 mmol, 0.5 equiv) in DMF (1 mL) followed by deprotection in TFA-CH2Cl2 essentially according to the procedure described in Example 27, Step C. Purification by reverse phase chromatography [95:5 water (+0.1% TFA)/CH3CN (+0.1% TFA) to 50:50 water (+0.1% TFA)/CH3CN (+0.1% TFA)] followed by lyophilization of the fractions afforded the title compound as a white powder. 1H NMR (400 MHz, CDCl3): δ 9.18 (s, 1 H), 8.45 (br s, 2 H), 8.00 (t, J=5.2 Hz, 1 H), 7.73 (d, J=2.0 Hz, 1 H), 7.41 (dd, J=2.0, 8.4 Hz, 1 H), 7.19 (d, J=8.4 Hz, 1 H), 4.41–4.34 (m, 2 H), 4.25 (dd, J=4.8, 14.8 Hz, 1 H), 4.00–3.94 (m, 1 H), 3.89–3.85 (m, 1 H), 3.53–3.46 (m, 1 H), 2.25–2.22 (m, 1 H), 2.09–1.85 (m, 5 H), 1.00 (s, 9 H). HRMS (APCI) M+H: calculated for (C20H28N7O2Cl)+ 434.2066, found 434.2065.

後処理

  1. customPurification by reverse phase chromatography [95:5 water (+0.1% TFA)/CH3CN (+0.1% TFA) to 50:50 water (+0.1% TFA)/CH3CN (+0.1% TFA)]

出典と根拠

ORDレコード
ord-1c55d26ea7694d1e93b820d18d71e1b4
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07144899B2

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