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Ammonia → 4-Amino-6-(4-iodophenyl)-7,8-dihydropyrimido[5,4-f][1,4]oxazepin-5(6H)-one

HRID 2237632
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HRID 2237632 반응식
Cl[C:2]1[C:7]2[C:8](=[O:20])[N:9]([C:13]3[CH:18]=[CH:17][C:16]([I:19])=[CH:15][CH:14]=3)[CH2:10][CH2:11][O:12][C:6]=2[N:5]=[CH:4][N:3]=1.CO.C(Cl)(Cl)Cl.[NH3:27]>O1CCOCC1>[NH2:27][C:2]1[C:7]2[C:8](=[O:20])[N:9]([C:13]3[CH:18]=[CH:17][C:16]([I:19])=[CH:15][CH:14]=3)[CH2:10][CH2:11][O:12][C:6]=2[N:5]=[CH:4][N:3]=1
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참가 물질

6

반응물 4

HCID 222AmmoniaHCID 887MethanolHCID 6212ChloroformHCID 593025014-chloro-6-(4-iodophenyl)-7,8-dihydropyrimido[5,4-f][1,4]oxazepin-5(6H)-one

생성물 1

HCID 593025304-Amino-6-(4-iodophenyl)-7,8-dihydropyrimido[5,4-f][1,4]oxazepin-5(6H)-one

시약·촉매·용매 1

HCID 312751,4-Dioxane
용매

실험 절차

A solution of 4-chloro-6-(4-iodophenyl)-7,8-dihydropyrimido[5,4-f][1,4]oxazepin-5(6H)-one (279 mg, 0.70 mmol) in 0.5 N ammonia in p-dioxane was stirred in a sealed tube for 18 hours. Concentration of the reaction mixture, followed by chromatography (10 g silica gel, 0-5% methanol: chloroform) afforded the title compound of Preparation 5 as a white solid, 122 mg. 1H NMR (400 MHz, DMSO-d6) δ 8.18 (s, 1H), 7.80 (d, 2H), 7.60 (br s, 2H), 7.19 (d, 2H), 4.60 (m, 2H), 3.96 (m, 2H). m/z=383.1 (M+1).

후처리

  1. customafforded

출처 및 근거

ORD 기록
ord-35597a62fecf4cb2b0b55c04ee1ffaaa
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07718645B2

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