Water → Losartan potassium salt

HRID 917008

반응식

HRID 917008 반응식
[CH3:1][CH2:2][CH2:3][CH2:4][C:5]1[N:9]([CH2:10][C:11]2[CH:12]=[CH:13][C:14]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][C:22]=3[C:23]3[N:27]=[N:26][NH:25][N:24]=3)=[CH:15][CH:16]=2)[C:8]([CH2:28][OH:29])=[C:7]([Cl:30])[N:6]=1.[OH-].[K+:32].O>C(O)(C)C.CCCCCCC>[CH3:1][CH2:2][CH2:3][CH2:4][C:5]1[N:9]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][C:22]=3[C:23]3[N:27]=[N:26][N-:25][N:24]=3)=[CH:13][CH:12]=2)[C:8]([CH2:28][OH:29])=[C:7]([Cl:30])[N:6]=1.[K+:32]

참가 물질

6

반응물 3

HCID 962WaterHCID 3961LosartanHCID 14797Potassium Hydroxide

생성물 1

HCID 11476710Losartan potassium salt수율 86.3%

시약·촉매·용매 2

HCID 3776Isopropanol용매2회HCID 8900Heptane용매

실험 절차

To 40.81 g losartan (chromatographic purity 98.73%) in 153 ml i-propanol, a mixture of 10 g potassium hydroxide, 5.1 ml water, and 100 ml i-propanol was added at a temperature of 38-40° C. to a pH of 10-11 during half an hour. Approximately 140 ml of the solvent (i-propanol/water mixture) were removed by distillation, and 92 ml n-heptane were added. It was stirred at room temperature until a white precipitate was formed. The precipitate was diluted with 54 ml n-heptane, filtered, washed with 70 ml n-heptane, and dried in vacuo at 50° C. to yield 38.4 g losartan potassium (yield: 86%, chromatographic purity: 99.67%).

후처리

  1. additionwas added at a temperature of 38-40° C. to a pH of 10-11 during half an hour
  2. customApproximately 140 ml of the solvent (i-propanol/water mixture) were removed by distillation, and 92 ml n-heptane
  3. additionwere added
  4. customwas formed
  5. filtrationfiltered
  6. washwashed with 70 ml n-heptane
  7. customdried in vacuo at 50° C.

출처 및 근거

ORD 기록
ord-7c7200f62ceb4fb18bc202156ba26898
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07271269B2

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