Methanol → HCID 178434787, 화합물

HRID 1639575노트

반응식

HRID 1639575 반응식
[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

참가 물질

5

반응물 4

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

생성물 1

HCID 178434787HCID 178434787, 화합물

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a01ec2e11f9b46d1b5adad909e8c5b13
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110577B2

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