Hydrochloric Acid → HCID 54025116、化合物

HRID 482702

反応式

HRID 482702 の反応式
[O:1]=[C:2]([CH2:4][N:5]([C:7](=[NH:9])[NH2:8])[CH3:6])[OH:3].[OH-].C([N+](CCCC)(CCCC)CCCC)CCC.[Cl:28][C:29]1[CH:30]=[C:31]([N:35]=[C:36]=[O:37])[CH:32]=[CH:33][CH:34]=1.Cl>CO.CN(C=O)C.O>[NH2:9][C:7](=[N:8][C:36]([NH:35][C:31]1[CH:32]=[CH:33][CH:34]=[C:29]([Cl:28])[CH:30]=1)=[O:37])[N:5]([CH3:6])[CH2:4][C:2]([OH:3])=[O:1]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 586CreatineHCID 17968Benzene, 1-chloro-3-isocyanato-HCID 2723671Tetrabutylammonium Hydroxide

生成物 1

HCID 54025116HCID 54025116、化合物収率 30%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of 9.58 g (0.073 mole) of anhydrous creatine in 96 ml (0.073 mole) of 0.76M tetrabutylammonium hydroxide in methanol was evaporated to an oil in vacuo. The residue was dissolved in 100 ml of DMF. An 11.2 g (0.073 mole) sample of m-chlorophenylisocyanate was added dropwise and the reaction was stirred for two hours. The mixture was poured into 200 ml of water and 73 ml of 1N HCl. The gummy precipitate was induced to crystallize by scratching. The solid was collected and triturated with tetrahydrofuran to give 6.6 g (30% yield) of light yellow solid N-{amino[(3-chlorophenyl)aminocarbonyl]iminomethyl}-N-methylglycine. A hydrochloride salt was prepared from conc. HCl to yield a pink solid, m.p. 228°-234° C.

後処理

  1. customto crystallize
  2. customThe solid was collected
  3. customtriturated with tetrahydrofuran

出典と根拠

ORDレコード
ord-388581ef70954789afe2084c405d230e
出典データセット
uspto-grants-1986_03
特許番号
US04575514

関連ノート

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