Water → Tert-butyl (6-iodoimidazo[1,2-b]pyridazin-2-yl)carbamate

HRID 1663617

반응식

HRID 1663617 반응식
[NH2:1][C:2]1[N:3]=[N:4][C:5]([I:8])=[CH:6][CH:7]=1.Cl[CH2:10][C:11]([NH:13][C:14](=[O:20])[O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=O.P([O-])([O-])(O)=O.[Na+].[Na+].O>CN(C)C(=O)C>[I:8][C:5]1[CH:6]=[CH:7][C:2]2[N:3]([CH:10]=[C:11]([NH:13][C:14](=[O:20])[O:15][C:16]([CH3:19])([CH3:18])[CH3:17])[N:1]=2)[N:4]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 24203Sodium Phosphate, DibasicHCID 108678346-Iodopyridazin-3-amineHCID 14221822HCID 14221822, 화합물

생성물 1

HCID 46941915Tert-butyl (6-iodoimidazo[1,2-b]pyridazin-2-yl)carbamate수율 63%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
120 °C

실험 절차

To a solution of 3-amino-6-iodopyridazine (10.0 g, 45.2 mmol) in N,N-dimethylacetamide (100 mL) were added tert-butyl (chloroacetyl)carbamate (14.0 g, 72.4 mmol) and disodium hydrogenphosphate (16.1 g, 113 mmol), and the mixture was stirred at 120° C. for 3 hr. After cooling the mixture to room temperature, water (400 mL) was added to the mixture, and the precipitated crystals were filtrated, and washed with acetonitrile and petroleum ether to give the title compound (10.2 g, 63%) as a green powder.

후처리

  1. temperatureAfter cooling the mixture to room temperature
  2. filtrationthe precipitated crystals were filtrated
  3. washwashed with acetonitrile and petroleum ether

출처 및 근거

ORD 기록
ord-a0e9ff83a97a417aa675e8332b54e6f3
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08034812B2

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