Water → HCID 54231516, 화합물

HRID 1900186

반응식

HRID 1900186 반응식
CN1CCOCC1.Cl[C:9]([O:11][CH:12]1[CH2:17][CH2:16][CH2:15][CH:14]([CH3:18])[CH2:13]1)=[O:10].[C:19]([C:21]1[CH:38]=[CH:37][C:24]([O:25][CH2:26][CH:27]([NH:29][C:30](=[O:36])[C@H:31]([CH:33]([CH3:35])[CH3:34])[NH2:32])[CH3:28])=[CH:23][CH:22]=1)#[N:20].O>C(Cl)Cl>[C:19]([C:21]1[CH:22]=[CH:23][C:24]([O:25][CH2:26][CH:27]([NH:29][C:30](=[O:36])[C@H:31]([CH:33]([CH3:34])[CH3:35])[NH:32][C:9]([O:11][CH:12]2[CH2:17][CH2:16][CH2:15][CH:14]([CH3:18])[CH2:13]2)=[O:10])[CH3:28])=[CH:37][CH:38]=1)#[N:20]

참가 물질

6

반응물 4

HCID 962WaterHCID 79724-MethylmorpholineHCID 127054633-Methylcyclohexyl chloroformateHCID 22866848N1-[2-(4-cyanophenoxy)-1-methylethyl]-L-valinamide

생성물 1

HCID 54231516HCID 54231516, 화합물수율 79.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

0.4 g of N-methylmorpholine, and subsequently 0.8 g of 3-methylcyclohexyl chloroformate were added to a suspension containing 1.0 g of N1 -[2-(4-cyanophenoxy)-1-methylethyl]-L-valinamide suspended in 50 ml of methylene chloride at -15° C. The mixture was allowed to sit and warm naturally to room temperature and stirred for 15 hours at room temperature. Water was subsequently added to the reaction mixture. After the methylene chloride layer was washed with water, the organic layer was dried over anhydrous magnesium sulfate and then the methylene chloride was removed under reduced pressure. The residue was purified by column chromatography on silica gel, thus obtaining 1.2 g of the desired product in the form of a white crystal (yield: 80% ).

후처리

  1. washAfter the methylene chloride layer was washed with water
  2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  3. customthe methylene chloride was removed under reduced pressure
  4. customThe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-79bb7633d08d424ba82796a3a8d2600e
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05574064

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