Sodium Nitrite → HCID 178477834、化合物

HRID 505549ノート

反応式

HRID 505549 の反応式
[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]

参加物

6

反応物 2

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

生成物 1

HCID 178477834HCID 178477834、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3d11ac6398654e5ca14a71d10799db7f
出典データセット
uspto-grants-2010_08
特許番号
US07781454B2

反応ノート

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