Ammonia → Cyclobutylmethylamine

HRID 476956

反応式

HRID 476956 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH:7]1([C:11]([NH2:13])=[O:12])[CH2:10][CH2:9][CH2:8]1.C1(C(Cl)=O)CCC1.N>C(OCC)C>[NH2:13][CH2:11][CH:7]1[CH2:10][CH2:9][CH2:8]1.[CH:7]1([C:11]([NH2:13])=[O:12])[CH2:10][CH2:9][CH2:8]1

参加物

7

反応物 4

HCID 222AmmoniaHCID 78705Cyclobutanecarbonyl chlorideHCID 1274476CyclobutanecarboxamideHCID 21226445Aluminium lithium hydride

生成物 2

HCID 409746CyclobutylmethylamineHCID 1274476Cyclobutanecarboxamide

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

(Aminomethyl)cyclobutane was prepared by lithium aluminum hydride reduction of cyclobutanecarboxamide according to the procedure of Shatkina, T. N.: Reutov, O. A., Dokl. Akad. Nauk. SSSR. (1975) 219:1148 [Chem. Abs. 82: 139453m]. Cyclobutanecarboxamide was prepared as follows: a solution of commercially available cyclobutanecarboxylic acid chloride (10 g) in ethyl ether (500 ml) was stirred at 0° while ammonia gas was introduced, resulting in a white precipitate. This material was collected by filtration and redissolved in 50 ml of ethanol/water (4:1, v/v). This solution was applied to a column containing 75 grams of AG 1-X8 ion exchange resin (hydroxide ion form) (obtained from Bio-Rad Company), and elution was continued with ethanol (1 liter). Evaporation of the eluate provided a quantitative yield (8.36 g) of cyclobutanecarboxamide.

後処理

  1. additionwas introduced
  2. customresulting in a white precipitate
  3. filtrationThis material was collected by filtration
  4. dissolutionredissolved in 50 ml of ethanol/water (4:1
  5. additioncontaining

出典と根拠

ORDレコード
ord-4cc0b2311df74178a0227e121489c24a
出典データセット
uspto-grants-1989_12
特許番号
US04886800

関連ノート

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