HCID 15086004, 화합물 → HCID 21256462, 화합물

HRID 635859노트

반응식

HRID 635859 반응식
[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

참가 물질

5

반응물 1

HCID 15086004HCID 15086004, 화합물

생성물 1

HCID 21256462HCID 21256462, 화합물수율 101%

시약·촉매·용매 3

HCID 14801Manganese dioxide촉매HCID 1140Toluene용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-79aad8076cb54545a3b087e9f2968385
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06191124B1

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