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1,1'-Carbonyldiimidazole → 3-(1-Phenylmethyl-2-pyrrolidinyl)phenyl 2-(4-morpholinyl)ethylcarbamate

HRID 742599
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HRID 742599 반응식
[C:1]1([CH2:7][N:8]2[CH2:12][CH2:11][CH2:10][CH:9]2[C:13]2[CH:14]=[C:15]([OH:19])[CH:16]=[CH:17][CH:18]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:20]([N:27]1[CH:31]=[CH:30][N:29]=[CH:28]1)(N1C=CN=C1)=[O:21].NCCN1C[CH2:39][O:38][CH2:37][CH2:36]1.C(=O)(O)[O-].[Na+]>O1CCCC1.C(O)(=O)C.CCOCC>[N:29]1([CH2:30][CH2:31][NH:27][C:20](=[O:21])[O:19][C:15]2[CH:16]=[CH:17][CH:18]=[C:13]([CH:9]3[CH2:10][CH2:11][CH2:12][N:8]3[CH2:7][C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[CH:14]=2)[CH2:28][CH2:39][O:38][CH2:37][CH2:36]1
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참가 물질

8

반응물 4

HCID 682631,1'-CarbonyldiimidazoleHCID 4082852-MorpholinoethylamineHCID 516892Sodium BicarbonateHCID 233612863-(1-Phenylmethyl-2-pyrrolidinyl)phenol

생성물 1

HCID 233613073-(1-Phenylmethyl-2-pyrrolidinyl)phenyl 2-(4-morpholinyl)ethylcarbamate수율 54%

시약·촉매·용매 3

HCID 176
Acetic Acid
용매
2회
HCID 3283Diethyl Ether용매
HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of 3-[1-phenylmethyl-2-pyrrolidinyl]phenol (0.64 g) in dry tetrahydrofuran (20 ml) was added 1,1'-carbonyldiimidazole (0.61 g) at ambient temperature, under nitrogen. The reaction mixture was stirred for 48 hrs, glacial acetic acid (0.50 ml) was added followed by a solution of 4-(2-aminoethyl)morpholine (0.43 ml) in tetrahydrofuran (1.0 ml) and glacial acetic acid (0.20 ml). After 3 hrs, the reaction mixture was poured into saturated sodium bicarbonate solution and ether. The layers were separated, and the aqueous phase was extracted with ether (2 times). The combined organic extracts were washed with saturated sodium bicarbonate and brine, dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated. The residue was purified by radial chromatography, using ether as the eluent. The appropriate fractions were collected and concentrated to give 0.56 g (54%) of product. Recrystallization from ether/petroleum ether gave the analytical sample, mp 74°-77° C.

후처리

  1. waitAfter 3 hrs
  2. customThe layers were separated
  3. extractionthe aqueous phase was extracted with ether (2 times)
  4. washThe combined organic extracts were washed with saturated sodium bicarbonate and brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated
  8. customThe residue was purified by radial chromatography
  9. customThe appropriate fractions were collected
  10. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8ad65e82c89e459ab691420507b771ae
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05554750

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