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2-Chlorobenzylamine → 2-(2-Chloro-benzylamino)-benzooxazol-6-ol

HRID 1988398
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HRID 1988398 반응식
Cl[C:2]1[O:3][C:4]2[CH:10]=[C:9]([OH:11])[CH:8]=[CH:7][C:5]=2[N:6]=1.[Cl:12][C:13]1[CH:20]=[CH:19][CH:18]=[CH:17][C:14]=1[CH2:15][NH2:16]>CN1C(=O)CCC1.C(OCC)(=O)C>[Cl:12][C:13]1[CH:20]=[CH:19][CH:18]=[CH:17][C:14]=1[CH2:15][NH:16][C:2]1[O:3][C:4]2[CH:10]=[C:9]([OH:11])[CH:8]=[CH:7][C:5]=2[N:6]=1
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참가 물질

5

반응물 2

HCID 666482-ChlorobenzylamineHCID 234412462-Chloro-1,3-benzoxazol-6-OL

생성물 1

HCID 577253862-(2-Chloro-benzylamino)-benzooxazol-6-ol

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

2-Chloro-benzooxazol-6-ol (1 eq) and 2-chloro-benzylamine (2 eq) was dissolved in NMP. Using a Personal Chemistry microwave system, the mixture was reacted at 180° C. for six minutes. The crude reaction mixture was diluted with ethyl acetate and washed once with brine and once with 1N HCl, or washed twice with brine, depending on the amine used. The organic layer was dried with anhydrous sodium sulfate, filtered and concentrated. This material was purified by silica gel column using hexane and ethyl acetate. MH+=275.1.

후처리

  1. customthe mixture was reacted at 180° C. for six minutes
  2. customThe crude reaction mixture
  3. washwashed once with brine and once with 1N HCl
  4. washwashed twice with brine
  5. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThis material was purified by silica gel column

출처 및 근거

ORD 기록
ord-a44c1871b5a94442b3ebb8fae14c4471
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07553854B2

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