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Phosgene → HCID 57842704、化合物

HRID 735593
ノート
印刷プレビュー

反応式

HRID 735593 の反応式
C(Cl)(Cl)=O.[NH2:5][C:6]1[CH:7]=[C:8]([C@@H:12]([NH:19][C:20]([O:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[O:21])[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:9]=[CH:10][CH:11]=1.[C:30]([O-:33])(O)=[O:31].[Na+].[Br:35][C:36]1[CH:41]=[CH:40][C:39]([CH2:42][CH2:43]O)=[C:38]([CH3:45])[CH:37]=1.[N-]=C=O.[H-].[Na+].[Cl-].[NH4+]>C1COCC1.O>[CH2:23]([O:22][C:20]([NH:19][C@H:12]([C:8]1[CH:9]=[CH:10][CH:11]=[C:6]([NH:5][C:30]([O:33][CH2:43][CH2:42][C:39]2[CH:40]=[CH:41][C:36]([Br:35])=[CH:37][C:38]=2[CH3:45])=[O:31])[CH:7]=1)[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:21])[C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 7

HCID 6371PhosgeneHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 105034IsocyanateHCID 516892Sodium BicarbonateHCID 57842670(S)-ethyl 3-(3-aminophenyl)-3-(benzyloxycarbonylamino)propanoateHCID 578428522-(4-Bromo-2-methylphenyl)ethanol

生成物

1
HCID 57842704HCID 57842704、化合物収率 57%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Phosgene (3.5 mmol, 1.75 mL, 20% in toluene) was added to a solution of 34C (600 mg, 1.75 mmol) and NaHCO3 (1.47 g, 17.5 mmol) at 0° C. After stirring for 1 h at rt, the solution was filtered and concentrated in vacuo. 30B (375 mg, 1.75 mmol) in THF (20 mL) was added to the crude isocyanate and the solution was cooled to −45° C. NaH (93 mg) was added in one portion and the mixture was warmed to 0° C. and stirred for 2 h at 0° C. and 15 h at ambient temperature. Ammonium chloride (5 mL, saturated) was added and the reaction mixture was diluted with water and extracted with EtOAc. The organics were combined, washed with brine, dried over Na2SO4 and concentrated in vacuo. The crude product was purified by flash chromatography (0% to 50% EtOAc in hexanes) to yield 34D (578 mg, 57%) as a yellow oil. 1H NMR (400 MHz, CDCl3) δ ppm 1.15 (t, J=7.15 Hz, 3 H) 2.32 (s, 3 H) 2.80-2.87 (m, J=6.87, 6.87 Hz, 2 H) 2.93 (t, J=7.15 Hz, 2 H) 4.05 (q, J=7.15 Hz, 2 H) 4.30 (t, J=7.15 Hz, 2 H) 5.02-5.18 (m, 3 H) 6.95-7.09 (m, 2 H) 7.23-7.37 (m, 10 H).

後処理

  1. filtrationthe solution was filtered
  2. concentrationconcentrated in vacuo
  3. temperaturethe solution was cooled to −45° C
  4. temperaturethe mixture was warmed to 0° C.
  5. stirringstirred for 2 h at 0° C. and 15 h at ambient temperature
  6. extractionextracted with EtOAc
  7. washwashed with brine
  8. dry with materialdried over Na2SO4
  9. concentrationconcentrated in vacuo
  10. customThe crude product was purified by flash chromatography (0% to 50% EtOAc in hexanes)

出典と根拠

ORDレコード
ord-ebc648b8ea664c5b92b74633ea085040
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07592331B2

反応ノート

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