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HRID1867953

反应详情

EQUATION

反应方程式

HRID 1867953 的结构方程式

REACTANTS

反应物

5
结构：O=C([O-])[O-].[Na+].[Na+]
HCID10340

Carbonic acid sodium salt (1:2)

CNa2O3

结构：Nc1nc2ccc(O)cc2s1
HCID33462

2-Amino-6-benzothiazolol

C7H6N2OS

2 次

结构：CCN(C(C)C)C(C)C
HCID81531

Diisopropylethylamine

C8H19N

结构：CC(C)(C)OC(=O)N1CCC(C(=O)O)CC1
HCID392871

1-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acid

C11H19NO4

结构：CN(C)C(On1nnc2cccnc21)=[N+](C)C.F[P-](F)(F)(F)(F)F
HCID9886157

Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

C10H15F6N6OP

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)N1CCC(C(=O)Nc2nc3ccc(O)cc3s2)CC1
HCID57980837

未命名化合物

收率 88.3%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：O
溶剂HCID962

Water

H2O

结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

2 次

PROCEDURE

实验过程

A solution of piperidine-1,4-dicarboxylic acid mono-tert-butyl ester (276 mg, 1.203 mmol), of HATU (549 mg, 1.444 mmol) and of diisopropylethylamine (187 mg, 1.44 mmol) in 3 ml of DMF is stirred at room temperature for 15 minutes. The 2-aminobenzothiazol-6-ol (intermediate 1) (200 mg, 1.203 mmol) dissolved in 3 ml of DMF is added in a single portion. The reaction medium is stirred at room temperature for 2 hours, poured into a 10% solution of Na2CO3 in water (20 ml) and extracted with ethyl acetate. The crude reaction product is purified by column chromatography (eluent: EtOAc/heptane (1/1)) to give 401 mg of 4-(6-hydroxybenzothiazol-2-ylcarbamoyl)-piperidine-1-carboxylic acid tert-butyl ester (white solid).

WORKUP

后处理

  1. additionis added in a single portion
  2. extractionextracted with ethyl acetate
  3. customThe crude reaction product
  4. customis purified by column chromatography (eluent: EtOAc/heptane (1/1))