Water → 1,1-Dimethylethyl (3-{[5-nitro-4-({4-[(phenylmethyl)oxy]phenyl}amino)-2-pyridinyl]oxy}phenyl)carbamate

https://huagongshe.com/reaction/1986380

참여 물질

역할	이름	HCID	투입량
반응물	Water	HCID 962	—
반응물	Sodium hydride	HCID 24758	—
반응물	tert-butyl N-(3-hydroxyphenyl)carbamate	HCID 312485	—
반응물	2-Chloro-5-nitro-N-{4-[(phenylmethyl)oxy]phenyl}-4-pyridineamine	HCID 86045153	—
용매	Dimethylformamide	HCID 6228	—
용매	Tetrahydrofuran	HCID 8028	—
생성물	1,1-Dimethylethyl (3-{[5-nitro-4-({4-[(phenylmethyl)oxy]phenyl}amino)-2-pyridinyl]oxy}phenyl)carbamate	HCID 86623350	92.1%

반응 조건

온도	60 °C

반응 단계

A solution of 1,1-Dimethylethyl (3-hydroxyphenyl)carbamate (7.05 g, 33.7 mmol) in THF (20 mL) was added dropwise to a suspension of NaH (60% dispersion in oil, 1.34 g, 33.7 mmol) in THF (50 mL). The product of Step 1 (12.0 g, 33.7 mmol) in DMF (100 mL) was then added and the mixture was heated to 60° C. overnight. The reaction mixture was then cooled, poured into H2O and extracted with EtOAc. The combined extracts were washed with brine, dried (MgSO4), filtered and the filtrates were concentrated to give the title compound as a yellow solid (16.4 g, 92%) which was used without purification. MS (ES+) m/e 529 [M+H]+.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US07547779B2
출처 데이터셋	uspto-grants-2009_06
ORD ID	ord-e5c19d13f6214901a1d89e66fa9700e1
출처 메모	uspto-grants-2009_06