HCID 21256450, 화합물 → 174209-00-8

HRID 635847노트

반응식

HRID 635847 반응식
[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

참가 물질

5

반응물 1

HCID 21256450HCID 21256450, 화합물

생성물 1

HCID 21256490174209-00-8수율 22.7%

시약·촉매·용매 3

HCID 14801Manganese dioxide촉매HCID 1140Toluene용매HCID 6228Dimethylformamide용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-1cfbedca2f9d430bab25174ce5e20675
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06191124B1

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