Methane → Losartan potassium salt

HRID 50114

반응식

HRID 50114 반응식
CC(CC(C)C)=O.[CH2:8]([C:12]1[N:13]([CH2:20][C:21]2[CH:26]=[CH:25][C:24]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=3[C:33]3[N:34]=[N:35][N:36](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:37]=3)=[CH:23][CH:22]=2)[C:14]([CH2:18][OH:19])=[C:15]([Cl:17])[N:16]=1)[CH2:9][CH2:10][CH3:11].[OH-].[K+:58].C>CO>[CH3:11][CH2:10][CH2:9][CH2:8][C:12]1[N:13]([CH2:20][C:21]2[CH:26]=[CH:25][C:24]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=3[C:33]3[N:37]=[N:36][N-:35][N:34]=3)=[CH:23][CH:22]=2)[C:14]([CH2:18][OH:19])=[C:15]([Cl:17])[N:16]=1.[K+:58]

참가 물질

5

반응물 3

HCID 297MethaneHCID 14797Potassium HydroxideHCID 698869092-n-butyl-4-chloro 1-[(2'-(2-triphenylmethyl-2H-tetrazol-5-yl)-1,1'biphenyl-4-yl)-me thyl]-1H-imidazol-5-methanol methyl-isobutyl ketone

생성물 1

HCID 11476710Losartan potassium salt수율 95.9%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

Under nitrogen, in a 500 ml flask a mixture of 175 ml of dry methanol, 20 g (0.026 mol) of 2-n-butyl-4-chloro 1-[(2′-(2-triphenylmethyl-2H-tetrazol-5-yl)-1,1′biphenyl-4-yl)-me thyl]-1H-imidazol-5-methanol methyl-isobutyl ketone solvate and 1.46 g (0.026 mol) of potassium hydroxide in 25 ml of methanol was warmed to reflux temperature over a period of 30 min. After refluxing for 4 h, the reaction was cooled to room temperature, treated with 0.6 g of charcoal and filtered. The filtrate was concentrated to a volume of 30-35 ml under diminished pressure, and after addition of 85 ml of acetonitrile again to a volume of 30-35 ml. After addition of further 85 ml of acetonitrile the solution is concentrated to a volume of 60-65 ml. The suspension was stirred at 0−(+)2° C. for 2 h, the precipitated crystals were filtered, washed three times with 30 ml of cold acetonitrile and dried at 70° C. to give 11.5 g (94%) of the title compound.

후처리

  1. temperaturewas warmed
  2. temperatureto reflux temperature over a period of 30 min
  3. temperatureAfter refluxing for 4 h
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated to a volume of 30-35 ml under diminished pressure
  6. additionafter addition of 85 ml of acetonitrile again to a volume of 30-35 ml
  7. additionAfter addition of further 85 ml of acetonitrile the solution
  8. concentrationis concentrated to a volume of 60-65 ml
  9. filtrationthe precipitated crystals were filtered
  10. washwashed three times with 30 ml of cold acetonitrile
  11. customdried at 70° C.

출처 및 근거

ORD 기록
ord-6022181667ea4138a8f6aead0a43b0a4
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710183B2

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