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1,2-Dichloroethane → [2-Methyl-2-({4-[2-(6-methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-quinoline-7-carbonyl}-amino)-propyl]-carbamic Acid Tert-Butyl Ester

HRID 8241
ノート
印刷プレビュー

反応式

HRID 8241 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([C:8]2[C:9]([C:16]3[C:25]4[C:20](=[CH:21][C:22]([C:26](O)=[O:27])=[CH:23][CH:24]=4)[N:19]=[CH:18][CH:17]=3)=[C:10]3[CH2:15][CH2:14][CH2:13][N:11]3[N:12]=2)[CH:5]=[CH:4][CH:3]=1.[C:29]([O:33][C:34](=[O:41])[NH:35][CH2:36][C:37]([NH2:40])([CH3:39])[CH3:38])([CH3:32])([CH3:31])[CH3:30].C(Cl)CCl.ON1C2C=CC=CC=2N=N1.C(N(CC)C(C)C)(C)C>ClCCl>[C:29]([O:33][C:34](=[O:41])[NH:35][CH2:36][C:37]([CH3:39])([NH:40][C:26]([C:22]1[CH:21]=[C:20]2[C:25]([C:16]([C:9]3[C:8]([C:6]4[CH:5]=[CH:4][CH:3]=[C:2]([CH3:1])[N:7]=4)=[N:12][N:11]4[CH2:13][CH2:14][CH2:15][C:10]=34)=[CH:17][CH:18]=[N:19]2)=[CH:24][CH:23]=1)=[O:27])[CH3:38])([CH3:32])([CH3:30])[CH3:31]
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 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 101337374-[2-(6-methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-quinoline-7-carboxylic acidHCID 17909918tert-butyl N-(2-amino-2-methylpropyl)carbamate

生成物 1

HCID 69365708
[2-Methyl-2-({4-[2-(6-methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-quinoline-7-carbonyl}-amino)-propyl]-carbamic Acid Tert-Butyl Ester
収率 91%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-[2-(6-methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-quinoline-7-carboxylic acid (0.16 g, 0.43 mmol), (2-amino-2-methyl-propyl)-carbamic acid tert-butyl ester (0.09 g, 0.47 mmol), EDC (0.09 g, 0.47 mmol), 1-hydroxybenzotriazole (0.06 g, 0.47 mmol) in dichloromethane (8.6 mL) is added N,N-diisopropylethylamine (0.25 mL, 1.29 mmol). The mixture is stirred at room temperature for 18 hand concentrated in vacuo. The residue is taken up in ethyl acetate, washed with water and saturated aqueous sodium chloride, dried over sodium sulfate and concentrated in vacuo. The residue is chromatographed on SiO2 (methanol/dichloromethane/2:98) to yield the title compound 0.21 g (91%) as a white solid.

後処理

  1. concentrationconcentrated in vacuo
  2. washwashed with water and saturated aqueous sodium chloride
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue is chromatographed on SiO2 (methanol/dichloromethane/2:98)

出典と根拠

ORDレコード
ord-30f0c1b87db9430091f5e9eccc27e8b7
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07087626B2

反応ノート

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