Toluene → N'-hydroxycyclohexanecarboximidamide

HRID 470651

反応式

HRID 470651 の反応式
Cl.[NH2:2][OH:3].C(=O)(O)[O-].[Na+].[CH:9]1([C:15]#[N:16])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.C1(C)C=CC=CC=1>C(O)(C)C>[OH:3][NH:2][C:15]([CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)=[NH:16]

参加物

6

反応物 4

HCID 1140TolueneHCID 69834CyanocyclohexaneHCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 178513282N'-hydroxycyclohexanecarboximidamide

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

To a solution of 1.9 g (27.4 mmol) of hydroxylamine hydrochloride in 22 mL of isopropyl alcohol, 3.3 g (40.3 mmol) of sodium bicarbonate was added. The resulting mixture was stirred at 25° C. to 30° C. for 10-15 min. 2.0 g (18.3 mmol) of cyclohexanecarbonitrile was added and stirred at 80° C. to 85° C. for 3-4 h. After the reaction period, the reaction mass was cooled to 25° C. to 30° C., filtered and washed with 10 mL of isopropyl alcohol. The filtrate was collected and distilled out completely to obtain a crude residue. The residue was chased with 5 mL of toluene, to yield the title compound.

後処理

  1. stirringstirred at 80° C. to 85° C. for 3-4 h
  2. customAfter the reaction period
  3. temperaturethe reaction mass was cooled to 25° C. to 30° C.
  4. filtrationfiltered
  5. washwashed with 10 mL of isopropyl alcohol
  6. customThe filtrate was collected
  7. distillationdistilled out completely
  8. customto obtain a crude residue

出典と根拠

ORDレコード
ord-95d1f5fc877e4904a3e837b3c0858057
出典データセット
uspto-grants-2014_01
特許番号
US08629277B2

関連ノート

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