HCID 21256507, 화합물 → HCID 21256465, 화합물

HRID 635867노트

반응식

HRID 635867 반응식
[CH3:1][O:2][C:3]1[CH:16]=[CH:15][C:6]2[N:7]3[C:12]([CH2:13][OH:14])=[CH:11][N:10]=[C:8]3[S:9][C:5]=2[CH:4]=1>CN(C=O)C.C1(C)C=CC=CC=1.O=[Mn]=O>[CH3:1][O:2][C:3]1[CH:16]=[CH:15][C:6]2[N:7]3[C:12]([CH:13]=[O:14])=[CH:11][N:10]=[C:8]3[S:9][C:5]=2[CH:4]=1

참가 물질

5

반응물 1

HCID 21256507HCID 21256507, 화합물

생성물 1

HCID 21256465HCID 21256465, 화합물수율 95.6%

시약·촉매·용매 3

HCID 14801Manganese dioxide촉매HCID 1140Toluene용매HCID 6228Dimethylformamide용매

실험 절차

A solution of 7-Methoxy-imidazo[2,1-b]benzothiazole-3-methanol (Formula M-2) (4.0 g) in DMF (25 mL) was diluted with toluene (200 mL) and the warm solution was treated with MnO2 (8.84 g). The suspension was azeotropically distilled for 4 hours, cooled to 50°, and filtered. The combined filtrate and toluene washes were concentrated and the concentrate was diluted with water. Precipitated 7-Methoxy-imidazo[2,1-b]benzothiazole-3-carboxaldehyde (Formula M-3) (3.8 g) was filtered and recrystallized from acetonitrile to yield pure 7-Methoxy-imidazo [2,1-b]benzothiazole-3-carboxaldehyde (Formula M-3) (3.79 g), m.p. 168-169°.

후처리

  1. distillationThe suspension was azeotropically distilled for 4 hours
  2. temperaturecooled to 50°
  3. filtrationfiltered
  4. concentrationThe combined filtrate and toluene washes were concentrated
  5. additionthe concentrate was diluted with water
  6. filtrationPrecipitated 7-Methoxy-imidazo[2,1-b]benzothiazole-3-carboxaldehyde (Formula M-3) (3.8 g) was filtered
  7. customrecrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-48770c2edb9f48eb91e30ec5cd6ab74e
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06191124B1

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