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Pyridine → (S)-3-(2-Benzyloxy-4-nitro-benzenesulfonylamino)-succinamic acid tert-butyl ester

HRID 1814344
ノート
印刷プレビュー

反応式

HRID 1814344 の反応式
C(Cl)Cl.[CH2:4]([O:11][C:12]1[CH:17]=[C:16]([N+:18]([O-:20])=[O:19])[CH:15]=[CH:14][C:13]=1[S:21](Cl)(=[O:23])=[O:22])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[C:25]([O:29][C:30](=[O:37])[CH2:31][C@H:32]([NH2:36])[C:33]([NH2:35])=[O:34])([CH3:28])([CH3:27])[CH3:26].N1C=CC=CC=1>C(OCC)(=O)C>[C:25]([O:29][C:30](=[O:37])[CH2:31][C@H:32]([NH:36][S:21]([C:13]1[CH:14]=[CH:15][C:16]([N+:18]([O-:20])=[O:19])=[CH:17][C:12]=1[O:11][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)(=[O:23])=[O:22])[C:33]([NH2:35])=[O:34])([CH3:28])([CH3:26])[CH3:27]
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 1049PyridineHCID 6344DichloromethaneHCID 7019655L-Aspartic alpha-amide beta-t-butyl esterHCID 225039842-Benzyloxy-4-nitro-benzenesulfonyl chloride

生成物 1

HCID 69692796(S)-3-(2-Benzyloxy-4-nitro-benzenesulfonylamino)-succinamic acid tert-butyl ester収率 43%

試薬・触媒・溶媒 1

HCID 8857
Ethyl Acetate
溶媒

実験手順

To a room temperature CH2Cl2 solution (50 mL) of 2-benzyloxy-4-nitro-benzenesulfonyl chloride from Route J (2.62 g, 8.0 mmol) was added (S)-3-amino-succinamic acid tert-butyl ester (1.50 g, 8.0 mmol) and pyridine (2.60 mL). The reaction mixture was allowed to stir for 12 h at room temperature. The reaction was then diluted with ethyl acetate (200 mL) and washed with 5% citric acid and then saturated NaHCO3. The organic phase was dried (MgSO4), and then the solvent was removed under vacuum. The resulting crude product was purified using silica gel flash chromatography (40% hexanes in EtOAc). (S)-3-(2-Benzyloxy-4-nitro-benzenesulfonylamino)-succinamic acid tert-butyl ester was obtained in 43% yield (1.66 g) as an off white foam. MS (APCI) m/z 478.3 (M−1).

後処理

  1. washwashed with 5% citric acid
  2. dry with materialThe organic phase was dried (MgSO4)
  3. customthe solvent was removed under vacuum
  4. customThe resulting crude product was purified

出典と根拠

ORDレコード
ord-cb860a1b13a44a35ad8528136398884d
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06875765B2

反応ノート

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