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Water → HCID 22283318, 화합물

HRID 1060296
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HRID 1060296 반응식
[CH3:1][O:2][C:3]1[C:8]2[N:9]=[C:10]([NH:12][C:13](=[O:15])[OH:14])[S:11][C:7]=2[C:6]([CH:16]=[CH2:17])=[CH:5][CH:4]=1.[OH2:18].C1C(=O)N([Br:26])C(=O)C1>C1COCC1>[Br:26][CH2:17][CH:16]([C:6]1[C:7]2[S:11][C:10]([NH:12][C:13](=[O:14])[OH:15])=[N:9][C:8]=2[C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)[OH:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 22283075HCID 22283075, 화합물

생성물 1

HCID 22283318HCID 22283318, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1.5 g of (4-methoxy-7-vinyl-benzothiazol-2-yl)-carbamic acid methyll ester (0.0057 Mol), dissolved in THF (60 ml) were treated with H2O (6 ml) and 1.0 g of NBS (0.006 Mol) at room temperature for 15 min. Then the solvent was removed, the residue taken up in H2O (30 ml) and extracted four times with ethyl acetate (50 ml). The combined organic phases were washed with brine and dried over MgSO4. After evaporation the crude product was subjected to column chromatography (silicagel, ethyl acetate). The title compound was obtained as a white solid (78%), F.p.: 150-155° C.

후처리

  1. customThen the solvent was removed
  2. extractionextracted four times with ethyl acetate (50 ml)
  3. washThe combined organic phases were washed with brine
  4. dry with materialdried over MgSO4
  5. customAfter evaporation the crude product

출처 및 근거

ORD 기록
ord-d961e430973c424fb9414fa216d999a9
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06521754B2

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