HCID 21256450、化合物 → 174209-00-8

HRID 635847ノート

反応式

HRID 635847 の反応式
[CH3:1][C:2]1[N:3]2[C:9]([CH2:10][OH:11])=[CH:8][N:7]=[C:4]2[S:5][CH:6]=1>CN(C=O)C.C1(C)C=CC=CC=1.O=[Mn]=O>[CH3:1][C:2]1[N:3]2[C:9]([CH:10]=[O:11])=[CH:8][N:7]=[C:4]2[S:5][CH:6]=1

参加物

5

反応物 1

HCID 21256450HCID 21256450、化合物

生成物 1

HCID 21256490174209-00-8収率 22.7%

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 3-Methylimidazo[2,1-b]thiazole-5-methanol (FIG. C-5) (0.9 g) in DMF (10 mL) was diluted with toluene (200 mL), treated with MnO2 (3.0), and azeotropically distilled for 1.5 hours. The suspension was filtered and the filtrate was concentrated to 10 mL. The concentrate was diluted with ice water and the precipitated 3-Methylimidazo[2,1-b]thiazole-5-carboxaldehyde (FIG. C-6) (0.665 g) was filtered. An aliquot (225 mg) was recrystallized from ethyl acetate-hexane to yield pure 3-Methylimidazo[2,1-b]thiazole-5-carboxaldehyde (FIG. C-6) (202 mg), m.p. 163-165°.

後処理

  1. distillationazeotropically distilled for 1.5 hours
  2. filtrationThe suspension was filtered
  3. concentrationthe filtrate was concentrated to 10 mL
  4. additionThe concentrate was diluted with ice water
  5. filtrationthe precipitated 3-Methylimidazo[2,1-b]thiazole-5-carboxaldehyde (FIG. C-6) (0.665 g) was filtered
  6. customAn aliquot (225 mg) was recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-1cfbedca2f9d430bab25174ce5e20675
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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