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HRID229809

反应详情

EQUATION

反应方程式

HRID 229809 的结构方程式

REACTANTS

反应物

2
结构：CC(=O)OI1(OC(C)=O)(OC(C)=O)OC(=O)c2ccccc21
HCID159087

Triacetoxyperiodinane

C13H13IO8

结构：CC(C)C[C@H](NC(=O)c1cc2ccccc2o1)C(=O)N[C@H]1CC[C@@H](C)N(S(=O)(=O)c2ccccn2)C[C@@H]1O
HCID16743099

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)C[C@H](NC(=O)c1cc2ccccc2o1)C(=O)N[C@H]1CC[C@@H](C)N(S(=O)(=O)c2ccccn2)CC1=O
HCID6918602

N-(1-Hydroxy-4-methyl-1-{[7-methyl-3-oxo-1-(pyridine-2-sulfonyl)azepan-4-yl]imino}pentan-2-yl)-1-benzofuran-2-carboximidic acid

C27H32N4O6S

收率 97%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

PROCEDURE

实验过程

Dess-Martin periodinane (0.077 g, 0.182 mmol) was added to a solution of Benzofuran-2-carboxylic acid {(S)-1-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-3-methyl-butyl}-amide (0.058 g, 0.107 mmol) in CH2Cl2 (10 ml) and was stirred at RT for 1 h. The solution was washed with 10% aq. Na2S2O3, then aq. sat. NaHCO3, then brine. Purification by column chromatography (50% to 80% ethyl acetate/hexanes) gave the title compound (0.056 g, 97%): 1H NMR: 8.72 (m, 1H), 8.0 (d, 1H), 8.92 (dd, 1H), 7.65 (d, 1H), 7.56 (d, 1H), 7.45 (s, 1H), 7.42 (dd, 2H), 7.28 (d, 1H), 7.10 (d, 1H), 5.15 (m, 1H), 4.77 (d, 1H), 4.68 (m, 1H), 4.40 (m, 1H), 3.86 (d, 1H), 2.20-2.08 (m, 2H), 1.78-1.50 (m, 5H), 1.22 (dd, 3H), 0.98 (m, 6H); Electrospray mass spec: M+H+=541.2.

WORKUP

后处理

  1. washThe solution was washed with 10% aq. Na2S2O3
  2. customPurification by column chromatography (50% to 80% ethyl acetate/hexanes)