Hydrochloric Acid → HCID 59199417, 화합물

HRID 2089530노트

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HRID 2089530 반응식
Cl.[CH3:2][O:3][C:4]([C:6]1[N:7]([CH:11]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14](O)([CH3:21])[CH2:13][C:12]2([CH3:24])[CH3:23])[CH:8]=[N:9][CH:10]=1)=[O:5]>CO>[CH3:2][O:3][C:4]([C:6]1[N:7]([CH:11]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14]([CH3:21])=[CH:13][C:12]2([CH3:24])[CH3:23])[CH:8]=[N:9][CH:10]=1)=[O:5]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 591994333-(4-hydroxy-2,2,4-trimethyl-1,2,3,4-tetrahydro-naphthalen-1-yl)-3H-imidazole-4-carboxylic acid methyl ester

생성물 1

HCID 59199417HCID 59199417, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
50 °C

실험 절차

To a 1.25 M anhydrous methanol solution of HCl (3 mL) is added 3-(4-hydroxy-2,2,4-trimethyl-1,2,3,4-tetrahydro-naphthalen-1-yl)-3H-imidazole-4-carboxylic acid methyl ester, which can be prepared as described in Example 38, (85 mg, 0.27 mmol). The reaction is then heated to 50° C., and is then concentrated to dryness. The resulting residue is purified by silica gel flash chromatography (diethylamine-methanol-dichloromethane, 0.5:1:98.5) to provide 3-(2,2,4-trimethyl-1,2-dihydro-naphthalen-1-yl)-3H-imidazole-4-carboxylic acid methyl ester; MS: (ESI) m/z 297.0 (M+H)+; 1H NMR (400 MHz, CDCl3) δ ppm 0.86 (s, 3 H), 1.13 (s, 3 H), 2.15 (d, J=1.3 Hz, 3 H), 3.91 (s, 3 H), 5.56 (s, 1 H), 6.31 (s, 1 H), 7.16-7.26 (m, 2 H), 7.31-7.41 (m, 2 H), 7.43 (s, 1 H), 7.70 (s, 1 H). The HCl salt of the title compound can be prepared by dissolution in diethyl ether followed by treatment with an excess of 1N HCl in diethyl ether. The resulting heterogeneous solution is concentrated to afford the HCl salt of 3-(2,2,4-trimethyl-1,2-dihydro-naphthalen-1-yl)-3H-imidazole-4-carboxylic acid methyl ester.

후처리

  1. customcan be prepared
  2. concentrationis then concentrated to dryness
  3. customThe resulting residue is purified by silica gel flash chromatography (diethylamine-methanol-dichloromethane, 0.5:1:98.5)

출처 및 근거

ORD 기록
ord-99bb2b2f88654c98afe3b2c912fff6f7
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08436035B2

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