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Bromine → 6-Amino-7-bromobenzothiazole

HRID 380612
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인쇄 미리보기

반응식

HRID 380612 반응식
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]2[N:6]=[CH:7][S:8][C:4]=2[CH:3]=1.[Br:11]Br.CCOC(C)=O.CCCCCC>CC(O)=O.CCOC(C)=O>[Br:11][C:3]1[C:4]2[S:8][CH:7]=[N:6][C:5]=2[CH:9]=[CH:10][C:2]=1[NH2:1]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 24408BromineHCID 682886-AminobenzothiazoleHCID 21226206Ethyl acetate hexane

생성물 1

HCID 47126206-Amino-7-bromobenzothiazole수율 80%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 8857Ethyl Acetate용매

반응 조건

온도
25 °C

실험 절차

To a solution of 6-aminobenzothiazole (16 g, 107 mmol) in 100 mL of AcOH was added Br2 (2.0 mL, 43 mmol) dropwise and the resulting reaction mixture was stirred for 1 h at 25° C. Reaction mixture was concentrated in vacuo, yielding a yellow solid which was dissolved in EtOAc and washed with aq. NaHCO3. Organic layer was dried over Na2SO4 and concentrated in vacuo, yielding an oil which was subjected to column chromatography (10-50% EtOAc/n-Hexane) to obtain 7.8 g (34 mmol, 80% ) of the desired product.

후처리

  1. customthe resulting reaction mixture
  2. customReaction mixture
  3. concentrationwas concentrated in vacuo
  4. customyielding a yellow solid which
  5. washwashed with aq. NaHCO3
  6. dry with materialOrganic layer was dried over Na2SO4
  7. concentrationconcentrated in vacuo
  8. customyielding an oil which

출처 및 근거

ORD 기록
ord-88a5e7a6c99342baa3100ee7104fb62c
출처 데이터셋
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06303643B1

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