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

HRID 1742268
ノート
印刷プレビュー

反応式

HRID 1742268 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 176
Acetic Acid
溶媒
2 回
HCID 3283Diethyl Ether溶媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0a95d265ee9d4b2890bd0e326fb6e9ef
出典データセット
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05338739

反応ノート

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