Water → Losartan potassium salt

HRID 917008

反応式

HRID 917008 の反応式
[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]

参加物

6

反応物 3

HCID 962WaterHCID 3961LosartanHCID 14797Potassium Hydroxide

生成物 1

HCID 11476710Losartan potassium salt収率 86.3%

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒2 回HCID 8900Heptane溶媒

実験手順

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%).

後処理

  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.

出典と根拠

ORDレコード
ord-7c7200f62ceb4fb18bc202156ba26898
出典データセット
uspto-grants-2007_09
特許番号
US07271269B2

関連ノート

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