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Tetrahydrofuran → HCID 68090528、化合物

HRID 554880
ノート
印刷プレビュー

反応式

HRID 554880 の反応式
[C:1]([O:5][C:6]([NH:8][C:9]1[S:10][C:11]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[C:12]([CH3:14])[N:13]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:20][C@@H:21]([CH3:24])[CH2:22]O.C1(P([C:38]2[CH:43]=[CH:42]C=CC=2)C2C=CC=CN=2)C=CC=CC=1.N(C(OCC)=O)=N[C:46]([O:48]CC)=[O:47].O1CCC[CH2:57]1>C(OCC)(=O)C>[C:1]([O:5][C:6]([N:8]([CH2:22][C@@H:21]([NH:20][C:46]([O:48][C:43]([CH3:42])([CH3:38])[CH3:57])=[O:47])[CH3:24])[C:9]1[S:10][C:11]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[C:12]([CH3:14])[N:13]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
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 8028TetrahydrofuranHCID 80307L-AlaninolHCID 220568ethyl N-ethoxycarbonyliminocarbamate2 回HCID 6218932-Pyridyldiphenylphosphine2 回HCID 53404548Ethyl 2-(tert-butoxycarbonylamino)-4-methylthiazole-5-carboxylate

生成物 1

HCID 68090528HCID 68090528、化合物
収率 78%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a mixture of ethyl 2-(tert-butoxycarbonylamino)-4-methylthiazole-5-carboxylate (0.29 g, 1.00 mmol), (S)-(+)-2-amino-1-propanol (0.18 g, 1.00 mmol) and diphenyl-2-pyridinylphosphine (0.40 g, 1.50 mmol) in anhydrous tetrahydrofuran (20.0 mL) was added diethyl azodicarboxylate (0.26 g, 1.50 mmol) at 0° C. The resulting solution was stirred at ambient temperature for 0.5 h. Additional diphenyl-2-pyridinylphosphine (0.13 g, 0.50 mmol) and diethyl azodicarboxylate (0.096 g, 0.50 mmol) were added to the reaction mixture and stirred at ambient temperature for 4 h. The reaction mixture was diluted with ethyl acetate (80 mL) and washed with 25% aqueous ammonium chloride solution (3×20 mL). The organic layer was dried over anhydrous sodium sulphate and filtered. The filtrate was concentrated in vacuo and the residue was purified by column chromatography eluted with 15-45% ethyl acetate in hexanes to afford the title compound as a colorless oil (0.35 g, 78%): 1H NMR (300 MHz, CDCl3) δ 5.30 (s, 1H), 4.26 (q, J=7.1 Hz, 2H), 4.18-3.95 (m, 3H), 2.59 (s, 3H), 1.58 (s, 9H), 1.33-1.28 (m, 12H), 1.17 (d, J=6.3 Hz, 3H); MS (ES+) m/z 244 (M−2Boc+1).

後処理

  1. stirringstirred at ambient temperature for 4 h
  2. washwashed with 25% aqueous ammonium chloride solution (3×20 mL)
  3. dry with materialThe organic layer was dried over anhydrous sodium sulphate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated in vacuo
  6. customthe residue was purified by column chromatography
  7. washeluted with 15-45% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-a2ad5e3539f3460ab6f554f2ff50a676
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08049016B2

反応ノート

読み込み中…

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