Hydrochloric Acid → HCID 54025116, 화합물

HRID 482702

반응식

HRID 482702 반응식
[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]

참가 물질

8

반응물 4

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

생성물 1

HCID 54025116HCID 54025116, 화합물수율 30%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-388581ef70954789afe2084c405d230e
출처 데이터셋
uspto-grants-1986_03
특허 번호
US04575514

연결된 노트

불러오는 중…