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Triethylamine → HCID 11401002、化合物

HRID 1955627
ノート
印刷プレビュー

反応式

HRID 1955627 の反応式
Cl.[CH:2]1([CH2:5][NH2:6])[CH2:4][CH2:3]1.[CH2:7](N(CC)CC)[CH3:8].[C:14]([N:21]1[CH:25]=[CH:24]N=C1)(N1C=CN=C1)=[O:15]>C(Cl)(Cl)Cl>[CH:2]1([CH2:5][NH:6][C:14]([NH:21][CH2:25][CH:24]2[CH2:8][CH2:7]2)=[O:15])[CH2:4][CH2:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 81671(Cyclopropylmethyl)ammonium chloride

生成物 1

HCID 11401002HCID 11401002、化合物収率 59.1%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Cyclopropanemethylamine hydrochloride (Aldrich, 1.00 g, 9.30 mmol) and triethylamine (0.95 g, 9.39 mmol) were dissolved in chloroform (10 mL). 1,1'-Carbonyldiimidazole (Aldrich, 0.754 g, 4.65 mmol) was added and the resulting solution maintained at ~55° C. for 22 h. The chloroform solution was extracted with 1N hydrochloric acid (2×50 mL) and then with water (50 mL) and dried. Evaporation of the chloroform gave crude product (650 mg) which was recrystallized from toluene to give 1,3-bis(cyclopropylmethyl)urea as white crystals (462 mg, 59%), m.p. 127°-130° C.; 1H-NMR (DMSO-d6) consistent with structure.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperaturethe resulting solution maintained at ~55° C. for 22 h
  2. extractionThe chloroform solution was extracted with 1N hydrochloric acid (2×50 mL)
  3. dry with materialwith water (50 mL) and dried
  4. customEvaporation of the chloroform
  5. customgave crude product (650 mg) which
  6. customwas recrystallized from toluene

出典と根拠

ORDレコード
ord-b83e3caf0aa04a61a4b73daa3af21c8b
出典データセット
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05776940

反応ノート

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