Sodium Nitrite → 4-(3-bromo-5-chlorophenoxy)-5-chloro-1H-1,2,3-benzotriazole

HRID 505522ノート

反応式

HRID 505522 の反応式
[Br:1][C:2]1[CH:3]=[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:19]([O-])=O.[Na+]>C(O)(=O)C.O.CCOC(C)=O>[Br:1][C:2]1[CH:3]=[C:4]([CH:15]=[C:16]([Cl:18])[CH:17]=1)[O:5][C:6]1[C:7]2[N:14]=[N:19][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 568337453-(3-Bromo-5-chlorophenoxy)-4-chlorobenzene-1,2-diamine

生成物 1

HCID 1784778354-(3-bromo-5-chlorophenoxy)-5-chloro-1H-1,2,3-benzotriazole

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-5-chlorophenoxy)-4-chlorobenzene-1,2-diamine (4.97 g, 14.3 mmol) in acetic acid (25 mL) was cooled to 15° C. under N2 and sodium nitrite (1.08 g, 15.7 mmol) in water (39.3 mL) was added dropwise. After 1.5 hours, the reaction was diluted with EtOAc (300 mL), and the organic phase was separated and washed with water (3×100 mL). The organic phase was then dried (MgSO4), filtered, concentrated to afford the title product. LRMS (M+1) 359.7.

後処理

  1. customthe organic phase was separated
  2. washwashed with water (3×100 mL)
  3. dry with materialThe organic phase was then dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-74226e5518c74d158f96955cd801b2e6
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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