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

HRID 582876노트

반응식

HRID 582876 반응식
[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]

참가 물질

6

반응물 4

HCID 947NitrogenHCID 24408Bromine2회HCID 158169243-Chloro-6-methoxy-1,2-benzoxazoleHCID 19595110CCl4 acetone

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매3회

실험 절차

To a stirred solution of 3-chloro-6-methoxy-1,2-benzisoxazole (25 g) in acetic acid (200 ml) was added to 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.

후처리

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

출처 및 근거

ORD 기록
ord-2e113e0fd1324768bc441ddb65972223
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925766

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