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Benzene, 2-fluoro-4-methyl-1-nitro- → (S)-3-(5-Methyl-2-nitro-phenylamino)-5-phenyl-pentanoic acid ethyl ester

HRID 1747292
ノート
印刷プレビュー

反応式

HRID 1747292 の反応式
F[C:2]1[CH:3]=[C:4]([CH3:11])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].Cl.[CH2:13]([O:15][C:16](=[O:28])[CH2:17][C@@H:18]([NH2:27])[CH2:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[CH3:14].CCN(C(C)C)C(C)C>CN(C=O)C.C(OCC)(=O)C>[CH2:13]([O:15][C:16](=[O:28])[CH2:17][C@@H:18]([NH:27][C:2]1[CH:3]=[C:4]([CH3:11])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9])[CH2:19][CH2:20][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)[CH3:14]
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 3

HCID 67966Benzene, 2-fluoro-4-methyl-1-nitro-HCID 81531DiisopropylethylamineHCID 67359326(S)-3-Amino-5-phenyl-pentanoic acid ethyl ester hydrochloride

生成物 1

HCID 59497545(S)-3-(5-Methyl-2-nitro-phenylamino)-5-phenyl-pentanoic acid ethyl ester収率 56.1%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

To a solution of 3-Fluoro-4-nitrotoluene (0.7 g, 4.5 mmol) in DMF (5 mL) were added (S)-3-Amino-5-phenyl-pentanoic acid ethyl ester hydrochloride (1.2 g, 4.5 mmol) and DIPEA (1.6 g, 9.0 mmol). The reaction mixture was stirred at room temperature for 48 h. The reaction mixture was then diluted with ethyl acetate and washed with water (×4). The organic phase was then dried over Na2SO4 and concentrated to afford an orange solid. The resulting residue was Purified by silica gel prep TLC using 4:1 Hexanes:ethyl acetate as an eluent to afford 0.9 g of the desired product.

後処理

  1. washwashed with water (×4)
  2. dry with materialThe organic phase was then dried over Na2SO4
  3. concentrationconcentrated
  4. customto afford an orange solid
  5. customThe resulting residue was Purified by silica gel prep TLC

出典と根拠

ORDレコード
ord-272b25c17459421388c7594fe89901f5
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09150556B2

反応ノート

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