Cyclamate → HCID 54245590、化合物

HRID 2071512

反応式

HRID 2071512 の反応式
[CH:1]1(NS(=O)(=O)O)CCCCC1.C[CH:13]([N:16]1[CH2:20][CH2:19][CH2:18][C:17]1=[NH:21])[CH2:14][CH3:15].[Cl:22][C:23]1[C:24]([CH3:32])=[C:25]([N:29]=[C:30]=[O:31])[CH:26]=[CH:27][CH:28]=1>>[CH2:13]([N:16]1[CH2:20][CH2:19][CH2:18][C:17]1=[N:21][C:30]([NH:29][C:25]1[CH:26]=[CH:27][CH:28]=[C:23]([Cl:22])[C:24]=1[CH3:32])=[O:31])[CH2:14][CH2:15][CH3:1]

参加物

4

反応物 3

HCID 7533CyclamateHCID 27357701-Chloro-3-isocyanato-2-methylbenzeneHCID 43121953HCID 43121953、化合物

生成物 1

HCID 54245590HCID 54245590、化合物

実験手順

The cyclohexylsulfamic acid salt of 1-2-butyl-2-iminopyrrolidine (7.99 g.; 0.025 mole) is converted to free base (3.5 g.; 0.025 mole) by adding 2.5 ml. of 50% NaOH to an aqueous slurry of the salt and benzene extraction. After drying over K2CO3, the benzene solution is filtered through diatomaceous earth and 4.19 g. (0.025 mole) of 3-chloro-2-methylphenylisocyanate is added. The reaction mixture is stirred at room temperature for 3 hours and then taken to dryness in vacuo to give an oily residue of 1-(1-n-butyl-2-pyrrolidylidene)-3-(3-chloro-2-methylphenyl)urea which is dissolved in ether and converted to the hydrochloride salt. Recrystallization from methanol-ether yields the product, 1-(1-n-butyl-2-pyrrolidylidene)-3-(3-chloro-2-methylphenyl)urea HCl hydrate, m.p. = 126°-128° C.

後処理

  1. additionby adding 2.5 ml
  2. extractionof 50% NaOH to an aqueous slurry of the salt and benzene extraction
  3. dry with materialAfter drying over K2CO3
  4. filtrationthe benzene solution is filtered through diatomaceous earth and 4.19 g

出典と根拠

ORDレコード
ord-8b393676e49f4fbfab14d476eb720879
出典データセット
uspto-grants-1977_09
特許番号
US04046909

関連ノート

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