Morpholine, hydrochloride (1:1) → Morpholine-4-carboximidamide hydrochloride

HRID 256712

反応式

HRID 256712 の反応式
C([NH:3][C:4]([NH:6][CH:7]1[CH2:9]C1)=[NH:5])#N.[ClH:10].N1CC[O:14][CH2:13][CH2:12]1>C(O)(C)C>[ClH:10].[N:6]1([C:4](=[NH:5])[NH2:3])[CH2:7][CH2:9][O:14][CH2:13][CH2:12]1

参加物

4

反応物 2

HCID 197884Morpholine, hydrochloride (1:1)HCID 178512341HCID 178512341、化合物

生成物 1

HCID 12427952Morpholine-4-carboximidamide hydrochloride収率 85%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
160 °C

実験手順

A mixture of 4.0 g (32.3 mmoles) of N-cyano-N'-cyclopropylguanidine and 3.98 g (32.3 mmoles) of morpholine hydrochloride is heated at 160° C. under a nitrogen atmosphere for 2 and a half hours. The solid mass obtained is dissolved in 200 ml of boiling isopropyl alcohol. The mixture is filtered hot and the filtrate is concentrated until a solid suspension appears. The mixture is then cooled to room temperature and 200 ml of diethyl ether are added. The reaction product crystallizes. It is filtered, washed with diethyl ether and dried. 6.8 g of N-]imino(cyclopropylamino)methyl]-4-morpholinecarboximidamide hydrochloride are obtained. Yield: 85%. M.P.: 195°-196° C.

後処理

  1. customThe solid mass obtained
  2. filtrationThe mixture is filtered hot
  3. concentrationthe filtrate is concentrated until a solid suspension
  4. temperatureThe mixture is then cooled to room temperature
  5. addition200 ml of diethyl ether are added
  6. customThe reaction product crystallizes
  7. filtrationIt is filtered
  8. washwashed with diethyl ether
  9. customdried

出典と根拠

ORDレコード
ord-e9d8d1c4b04e4b0ab4dc23ddc55eab85
出典データセット
uspto-grants-1993_11
特許番号
US05258513

関連ノート

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