Nitrogen → 7-Bromo-3-chloro-6-methoxy-1,2-benzisoxazole

HRID 2396725ノート

反応式

HRID 2396725 の反応式
[Cl:1][C:2]1[C:6]2[CH:7]=[CH:8][C:9]([O:11][CH3:12])=[CH:10][C:5]=2[O:4][N:3]=1.[Br:13]Br.N#N.CC(C)=O.C(Cl)(Cl)(Cl)Cl>C(O)(=O)C>[Br:13][C:10]1[C:5]2[O:4][N:3]=[C:2]([Cl:1])[C:6]=2[CH:7]=[CH:8][C:9]=1[O:11][CH3:12]

参加物

6

反応物 4

HCID 947NitrogenHCID 24408Bromine2 回HCID 158169243-Chloro-6-methoxy-1,2-benzoxazoleHCID 19595110CCl4 acetone

生成物 1

HCID 187964507-Bromo-3-chloro-6-methoxy-1,2-benzisoxazole

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒3 回

実験手順

To a stirred solution of 3-chloro-6-methoxy-1,2-benzisoxazole (25 g) in acetic acid (200 ml) was added a solution of bromine (32.6 g) in acetic acid (100 ml) dropwise under N2 at ambient temperature. The mixture was allowed to stir overnight. TLC (silica gel, 5% acetone/CCl4) revealed the presence of starting material. Additional bromine (11 g) in acetic acid (50 ml) was added, and the reaction mixture was allowed to stir overnight. The reaction was filtered and washed with water. The precipitate was collected and recrystallized from methanol to yield the desired compound, m.p. 134°-135° C.

後処理

  1. stirringto stir overnight
  2. filtrationThe reaction was filtered
  3. washwashed with water
  4. customThe precipitate was collected
  5. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-0172d78220634b63bd25f3290f1bb457
出典データセット
uspto-grants-1996_02
特許番号
US05494908

反応ノート

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