Hydrochloric Acid → 2'-(1H-Tetrazol-5-yl)-1,1'-biphenyl-4-carboxaldehyde (Losartan Impurity)

HRID 644925노트

반응식

HRID 644925 반응식
C([O:3][CH:4](OCC)[C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[C:17]2[N:18]=[N:19][N:20](C3CCCCO3)[N:21]=2)=[CH:7][CH:6]=1)C.C(O)C.Cl>O>[NH:21]1[C:17]([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[C:8]2[CH:9]=[CH:10][C:5]([CH:4]=[O:3])=[CH:6][CH:7]=2)=[N:18][N:19]=[N:20]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 586182215-(4'-diethoxymethyl-biphenyl-2-yl)-2-(tetrahydropyran-2-yl)-2H-tetrazole

생성물 1

HCID 1785194042'-(1H-Tetrazol-5-yl)-1,1'-biphenyl-4-carboxaldehyde (Losartan Impurity)

시약·촉매·용매 1

HCID 962Water용매

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온도
45 °C

실험 절차

To 5-(4′-diethoxymethyl-biphenyl-2-yl)-2-(tetrahydropyran-2-yl)-2H-tetrazole (0.408 g; 1.00 mmol) are added 94% ethanol (2.5 mL) and a 2N aqueous solution of hydrochloric acid (0.5 mL; 1.0 mmol). The resulting solution is heated to 45° C. for 3 hours. After the addition of water (about 2 mL) the mixture is allowed to cool down to room temperature and then stirred at 0 to 5° C. for 30 minutes. The resulting suspension is filtered and the solids are washed with a small amount of water, dried in vacuo at 40° C. to afford 2′-(1H-tetrazol-5-yl)biphenyl-4-carbaldehyde as white, crystalline powder.

후처리

  1. temperatureto cool down to room temperature
  2. filtrationThe resulting suspension is filtered
  3. washthe solids are washed with a small amount of water
  4. customdried in vacuo at 40° C.

출처 및 근거

ORD 기록
ord-462ebbd455dc47a788eeacbc2dd370a6
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700784B2

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