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1,2-Dichloroethane → N-(7'-bromo-4'-fluoro-2'-methoxy-5,6-dihydrospiro[[1,3]oxazine-4,9'-xanthene]-2-yl)-4-nitrobenzamide

HRID 931595
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HRID 931595 반응식
[NH2:1][C:2]1([CH2:20][CH2:21][OH:22])[C:15]2[CH:14]=[C:13]([O:16][CH3:17])[CH:12]=[C:11]([F:18])[C:10]=2[O:9][C:8]2[C:3]1=[CH:4][C:5]([Br:19])=[CH:6][CH:7]=2.[N+:23]([C:26]1[CH:36]=[CH:35][C:29]([C:30]([N:32]=[C:33]=S)=[O:31])=[CH:28][CH:27]=1)([O-:25])=[O:24].C(Cl)CCl.O>C1COCC1>[Br:19][C:5]1[CH:4]=[C:3]2[C:8]([O:9][C:10]3[C:11]([F:18])=[CH:12][C:13]([O:16][CH3:17])=[CH:14][C:15]=3[C:2]32[CH2:20][CH2:21][O:22][C:33]([NH:32][C:30](=[O:31])[C:29]2[CH:28]=[CH:27][C:26]([N+:23]([O-:25])=[O:24])=[CH:36][CH:35]=2)=[N:1]3)=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 962WaterHCID 1413984-Nitrobenzoyl isothiocyanateHCID 673827982-(9-amino-7-bromo-4-fluoro-2-methoxy-9H-xanthen-9-yl)ethanol

생성물 1

HCID 67439840N-(7'-bromo-4'-fluoro-2'-methoxy-5,6-dihydrospiro[[1,3]oxazine-4,9'-xanthene]-2-yl)-4-nitrobenzamide수율 56.8%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

To a solution of 2-(9-amino-7-bromo-4-fluoro-2-methoxy-9H-xanthen-9-yl)ethanol (7.17 g, 19.47 mmol) in THF (100 mL) was added 4-nitrobenzoyl isothiocyanate (4.26 g, 20.45 mmol). The reaction mixture was stirred for 30 min at RT. EDC (5.60 g, 29.2 mmol) and TEA (0.543 ml, 3.89 mmol) were added sequentially and the reaction mixture was heated to 70° C. for 1 hr. The reaction mixture was cooled to RT and water (50 ml) was added. The reaction mixture was stirred for 1 hr, upon which a precipitate formed, which was filtered off and washed with water and MeOH. The solid was dried to afford N-(7′-bromo-4′-fluoro-2′-methoxy-5,6-dihydrospiro[[1,3]oxazine-4,9′-xanthene]-2-yl)-4-nitrobenzamide (6.0 g, 11.06 mmol, 56.8% yield).

후처리

  1. temperaturethe reaction mixture was heated to 70° C. for 1 hr
  2. temperatureThe reaction mixture was cooled to RT
  3. stirringThe reaction mixture was stirred for 1 hr, upon which a precipitate
  4. customformed
  5. filtrationwhich was filtered off
  6. washwashed with water and MeOH
  7. customThe solid was dried

출처 및 근거

ORD 기록
ord-2824dfc552a142cca0ddf8243431f694
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296759B2

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