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HRID893052

反应详情

EQUATION

反应方程式

HRID 893052 的结构方程式

REACTANTS

反应物

1
结构：CC(C)(C)OC(=O)N1C[C@@H](N=[N+]=[N-])C[C@H]1C(=O)O
HCID12094910

(2S,4S)-1-Boc-4-azidopyrrolidine-2-carboxylic acid

C10H16N4O4

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)N1C[C@@H](N)C[C@H]1C(=O)O
HCID14842624

(4S)-4-Amino-1-(tert-butoxycarbonyl)-L-proline

C10H18N2O4

收率 91.1%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CCO.O
溶剂HCID19096565

未命名化合物

PROCEDURE

实验过程

Azido acid 5b (1.10 g, 4.29 mmol) was dissolved in 100 ml 10% water/ethanol containing 150 mg Pd/C and hydrogenated at 100 psi for 16 h. The mixture was filtered through a pad of celite, washed with 50 mL of 1:1 water/ethanol and the filtrate concentrated to dryness. This material was recrystallized from water/ethanol to give 900 mg of 6 (84% yield), m.p.=225°-227° C. (decomp.) 1H NMR (D2O) δ 1.40/1.44 (m, 9H), 2.11 (m, 1H), 2.68 (m, 1H), 3.69 (m, 2H), 3.99 (m, 2H), 4.20 (dd, J=9.0/3.9 Hz, 1H). Anal. (C10H18N2O4.H2O) C, H, N.

WORKUP

后处理

  1. filtrationThe mixture was filtered through a pad of celite
  2. washwashed with 50 mL of 1:1 water/ethanol
  3. concentrationthe filtrate concentrated to dryness
  4. customThis material was recrystallized from water/ethanol