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

HRID 1922195ノート

反応式

HRID 1922195 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c3dbcecbbb72402dafc5054673158991
出典データセット
uspto-grants-2012_05
特許番号
US08173689B2

反応ノート

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