HCID 15086004、化合物 → HCID 21256462、化合物

HRID 635859ノート

反応式

HRID 635859 の反応式
[N:1]1[CH:2]=[C:3]([CH2:13][OH:14])[N:4]2[C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=3[S:6][C:5]=12>CN(C=O)C.C1(C)C=CC=CC=1.O=[Mn]=O>[N:1]1[CH:2]=[C:3]([CH:13]=[O:14])[N:4]2[C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=3[S:6][C:5]=12

参加物

5

反応物 1

HCID 15086004HCID 15086004、化合物

生成物 1

HCID 21256462HCID 21256462、化合物収率 101%

試薬・触媒・溶媒 3

HCID 14801Manganese dioxide触媒HCID 1140Toluene溶媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of imidazo[2,1-b]benzothiazole-3-methanol (Formula J-2) (2.0 g) in DMF (30 mL) and toluene (200 mL) was treated with MnO2 (4.5 g) and the mixture was azeotropically distilled for 4.5 hours. A second change of MnO2 (2.0 g) and distillation for 1 hour completed the conversion. The suspension was filtered, the combined filtrate and ethyl acetate washes of the cake were concentrated, the residue was diluted with water, and filtered to yield imidazo[2,1-b]benzothiazole-3-carboxaldehyde (Formula J-3) (2.0 g). Crude imidazo[2,1-b]benzothiazole-3-carboxaldehyde (Formula J-3) was used without further purification.

後処理

  1. distillationthe mixture was azeotropically distilled for 4.5 hours
  2. distillationA second change of MnO2 (2.0 g) and distillation for 1 hour
  3. filtrationThe suspension was filtered
  4. concentrationthe combined filtrate and ethyl acetate washes of the cake were concentrated
  5. additionthe residue was diluted with water
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-79aad8076cb54545a3b087e9f2968385
出典データセット
uspto-grants-2001_02
特許番号
US06191124B1

反応ノート

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