N-Methyl-1,3-propanediamine → 2-Diphenylmethylamino-1,4,5,6-tetrahydro-1-methylpyrimidine Hydroiodide

HRID 46635노트

반응식

HRID 46635 반응식
[IH:1].[C:2]1([CH:8]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[NH:9][C:10](=[NH:13])SC)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:20][NH:21][CH2:22][CH2:23][CH2:24]N>ClC1C=CC=CC=1Cl>[IH:1].[C:2]1([CH:8]([NH:9][C:10]2[N:21]([CH3:20])[CH2:22][CH2:23][CH2:24][N:13]=2)[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 80511N-Methyl-1,3-propanediamineHCID 178504030HCID 178504030, 화합물

생성물 1

HCID 202981512-Diphenylmethylamino-1,4,5,6-tetrahydro-1-methylpyrimidine Hydroiodide

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

실험 절차

To 38.43 grams (0.10 mole) of 1-diphenylmethyl-2-methyl-2-thiopseudourea hydroiodide in 270 milliliters of o-dichlorobenzene was added 8.81 grams (0.10 mole) of N-methyl-1,3-diaminopropane, and the resulting mixture was allowed to reflux for about 21 hours to produce the desired 2-diphenylmethylamino-1,4,5,6-tetrahydro-1-methylpyrimidine product. Thereafter, the mixture was allowed to cool, the solvent was decanted off and isopropanol was added to the residue to obtain 35.0 grams (86 percent yield) of a 2-diphenylmethylamino-1,4,5,6-tetrahydro-1-methylpyrimidine hydroiodide salt. After successive recrystallizations from acetone-ether and acetone-isopropanol, a purified product was obtained having a melting point (151°) 169°-171° C.

후처리

  1. temperatureto reflux for about 21 hours

출처 및 근거

ORD 기록
ord-ad1558a8b058489db8b03db88cafce92
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04174401

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