Potassium Carbonate → tert-Butyl (+)-(1-{2-[4-Benzoyl-2-(3,4-difluorophenyl)morpholin-2-yl]ethyl}-4-phenylpiperid-4-yl)carbamate

HRID 1937036노트

반응식

HRID 1937036 반응식
C(=O)([O-])[O-].[K+].[K+].Cl.[C:8]1([C:14]2([NH:20][C:21](=[O:27])[O:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[C:28]([N:36]1[CH2:41][CH2:40][O:39][C:38]([C:54]2[CH:59]=[CH:58][C:57]([F:60])=[C:56]([F:61])[CH:55]=2)([CH2:42][CH2:43]OS(C2C=CC=CC=2)(=O)=O)[CH2:37]1)(=[O:35])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>O.C(#N)C>[C:28]([N:36]1[CH2:41][CH2:40][O:39][C:38]([CH2:42][CH2:43][N:17]2[CH2:18][CH2:19][C:14]([NH:20][C:21](=[O:27])[O:22][C:23]([CH3:24])([CH3:26])[CH3:25])([C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH2:15][CH2:16]2)([C:54]2[CH:59]=[CH:58][C:57]([F:60])=[C:56]([F:61])[CH:55]=2)[CH2:37]1)(=[O:35])[C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 11179272(+)-4-Benzoyl-2-(3,4-difluorophenyl)-2-(2-benzenesulfonyloxyethyl)morpholineHCID 86758087Tert-butyl (4-phenylpiperid-4-yl)carbamate hydrochloride2회

생성물 1

HCID 9916832tert-Butyl (+)-(1-{2-[4-Benzoyl-2-(3,4-difluorophenyl)morpholin-2-yl]ethyl}-4-phenylpiperid-4-yl)carbamate

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

반응 조건

온도
70 °C

실험 절차

A solution of 18 g of potassium carbonate in 18 ml of water is added to a mixture of 22.6 g of tert-butyl (4-phenylpiperid-4-yl)carbamate hydrochloride (compound (IV)) and 30 g of compound of formula (III) obtained in Example 1 in 300 ml of acetonitrile, and the mixture is then heated at 70° C. for 12 hours and left overnight at room temperature. The acetonitrile is concentrated under vacuum, the residue is taken up in 300 ml of dichloromethane, the organic phase is washed successively with 150 ml of a 0.3 M solution of sodium hydroxide in water, with 150 ml of water, twice with 150 ml of pH 2 sulfate buffer, with 150 ml of water and with 150 ml of a 10% by weight solution of potassium carbonate in water, dried over magnesium sulfate and filtered, and the solvent is evaporated off under vacuum at room temperature. The expected product is obtained, which is used in Example 3.

후처리

  1. concentrationThe acetonitrile is concentrated under vacuum
  2. washthe organic phase is washed successively with 150 ml of a 0.3 M solution of sodium hydroxide in water, with 150 ml of water, twice with 150 ml of pH 2 sulfate buffer, with 150 ml of water and with 150 ml of a 10% by weight solution of potassium carbonate in water
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customthe solvent is evaporated off under vacuum at room temperature

출처 및 근거

ORD 기록
ord-ce307eb3c7754bd1af7dce4a914f4fc8
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06392039B1

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