4,5-Dimethyl-1,2-phenylenediamine → 2-Butyl-5,6-dimethyl-1H-benzimidazole

반응식

[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([NH2:9])=[C:4]([NH2:10])[CH:3]=1.Cl.[C:12](=N)(OCC)[CH2:13][CH2:14][CH2:15][CH3:16]>>[CH2:13]([C:12]1[NH:10][C:4]2[CH:3]=[C:2]([CH3:1])[C:7]([CH3:8])=[CH:6][C:5]=2[N:9]=1)[CH2:14][CH2:15][CH3:16]

참가 물질

반응물 2

HCID 766354,5-Dimethyl-1,2-phenylenediamine

HCID 12283341Ethyl pentanimidate hydrochloride

생성물 1

HCID 149873242-Butyl-5,6-dimethyl-1H-benzimidazole수율 74.9%

실험 절차

Using the procedure of Step A of Example 1, 2.04 g of 4,5-dimethyl-1,2-phenylene diamine and 3.73 g of ethyl pentanimidoate hydrochloride [J.A.C.S., Vol. 64, p. 1827 (1942)] were reacted to obtain 3.48 g of crude product which was chromatographed on silica (eluant: methylene chloride-methanol (9-1)) to obtain 2.27 g of the expected compound melting at 110° C. An analytical sample was prepared by crystallization of 120 mg of the product from isopropyl ether to obtain 88 mg of product melting at 110° C.

후처리

customwere reacted
customto obtain 3.48 g of crude product which
customwas chromatographed on silica (eluant: methylene chloride-methanol (9-1))

출처 및 근거

ORD 기록: ord-094b8f584b5e450ca83d4a2bf782c4b6
출처 데이터셋: uspto-grants-1995_11
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05470867

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