Sodium Nitrite → HCID 178477834, 화합물

HRID 505549노트

반응식

HRID 505549 반응식
[Br:1][C:2]1[C:3]([Cl:19])=[C:4]([CH:15]=[C:16]([Cl:18])[CH:17]=1)[O:5][C:6]1[C:11]([Cl:12])=[CH:10][CH:9]=[C:8]([NH2:13])[C:7]=1[NH2:14].[N:20]([O-])=O.[Na+]>C(O)(=O)C.O.CCOC(C)=O>[Br:1][C:2]1[C:3]([Cl:19])=[C:4]([CH:15]=[C:16]([Cl:18])[CH:17]=1)[O:5][C:6]1[C:7]2[N:14]=[N:20][NH:13][C:8]=2[CH:9]=[CH:10][C:11]=1[Cl:12]

참가 물질

6

반응물 2

HCID 23668193Sodium NitriteHCID 684264093-(3-Bromo-2,5-dichlorophenoxy)-4-chlorobenzene-1,2-diamine

생성물 1

HCID 178477834HCID 178477834, 화합물

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

3-(3-bromo-2,5-dichlorophenoxy)-4-chlorobenzene-1,2-diamine (2.48 g, 6.47 mmol) in acetic acid (20 mL) was cooled to 15° C., after which sodium nitrite (0.446 g, 6.47 mmol) in water (6.47 mL) was added dropwise under N2. After 1.5 hours, the reaction mixture was diluted with EtOAc (200 mL), and the organic phase was separated and washed with water (3×75 mL). The organic phase was dried (MgSO4), filtered, concentrated and placed under vacuum to yield the title compound. LRMS (M+1)=393.4.

후처리

  1. customthe organic phase was separated
  2. washwashed with water (3×75 mL)
  3. dry with materialThe organic phase was dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3d11ac6398654e5ca14a71d10799db7f
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07781454B2

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