Methanol → HCID 178434787、化合物

HRID 1639575ノート

反応式

HRID 1639575 の反応式
[C:1]1([NH:7][C:8](=[O:23])[CH:9]([C:17]2[S:21][N:20]=[C:19]([CH3:22])[N:18]=2)[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15]#[N:16])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO.[OH2:26].[NH2:27]O.O>>[C:1]1([NH:7][C:8](=[O:23])[CH:9]([C:17]2[S:21][N:20]=[C:19]([CH3:22])[N:18]=2)[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15](=[NH:27])[NH:16][OH:26])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 4

HCID 887MethanolHCID 962WaterHCID 22235265Hydroxylamine monohydrateHCID 593780587-Cyano-2-(3-methyl[1,2,4]thiadiazol-5-yl)heptanoic acid phenylamide

生成物 1

HCID 178434787HCID 178434787、化合物

実験手順

To a stirred mixture of 7-cyano-2-(3-methyl[1,2,4]thiadiazol-5-yl)heptanoic acid phenylamide (2021044) (440 mg, 1.30 mmol) in 50% hydroxylamine/water (20 mL) was added methanol until the oil dissolved. The solution was then heated at reflux overnight. Water (100 mL) was added and the reaction mixture was then extracted with ethyl acetate (3×150 mL). The combined organic fractions were dried (MgSO4) and the solvent was removed under reduced pressure. The crude product (400 mg, 1.1 mmol) was purified by preparative liquid chromatography to afford 7-(N-hydroxycarbamimidoyl)-2-(3-methyl-[1,2,4]thiadiazol-5-yl)-heptanoic acid phenylamide (2021035) as a white solid.

後処理

  1. dissolutiondissolved
  2. temperatureThe solution was then heated
  3. temperatureat reflux overnight
  4. extractionthe reaction mixture was then extracted with ethyl acetate (3×150 mL)
  5. dry with materialThe combined organic fractions were dried (MgSO4)
  6. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-a01ec2e11f9b46d1b5adad909e8c5b13
出典データセット
uspto-grants-2012_02
特許番号
US08110577B2

反応ノート

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