Hydrochloric Acid → HCID 178478959, 화합물

HRID 1512169노트

반응식

HRID 1512169 반응식
[O:1]1[CH2:6][CH2:5][CH:4](/[CH:7]=[CH:8]/[C:9]2[NH:13][C:12]3[CH:14]=[CH:15][C:16]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=4[C:24]([F:27])([F:26])[F:25])=[CH:17][C:11]=3[N:10]=2)[CH2:3][CH2:2]1.[ClH:28].CC(O)C>CCO>[ClH:28].[O:1]1[CH2:6][CH2:5][CH:4](/[CH:7]=[CH:8]/[C:9]2[NH:13][C:12]3[CH:14]=[CH:15][C:16]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=4[C:24]([F:25])([F:26])[F:27])=[CH:17][C:11]=3[N:10]=2)[CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 178506129HCID 178506129, 화합물

생성물 1

HCID 178478959HCID 178478959, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of (E)-2-[2-(tetrahydro-pyran-4-yl)-vinyl]-5-(2-trifluoromethyl-phenyl)-1H-benzimidazole (0.220 g, 0.591 mmol, prepared as in STEP D above) in EtOH (4 mL) was treated with 5M HCl in i-PrOH (130 μL, 0.650 mmol) at room temperature for 1 h and concentrated in vacuo. The residue was taken up in a minimum amount of EtOH (2 mL). Hexane was added with stirring until the mixture became cloudy. EtOH (1 mL) was added, and hexane was very slowly added until precipitate formed. The resulting mixture was cooled in the refrigerator for 45 min. The solid was filtered, washed with cold hexane, and air-dried to yield (E)-2-[2-(tetrahydro-pyran-4-yl)-vinyl]-5-(2-trifluoromethyl-phenyl)-1H-benzimidazole hydrochloride as an off-white solid.

후처리

  1. concentrationconcentrated in vacuo
  2. additionHexane was added
  3. additionEtOH (1 mL) was added
  4. additionhexane was very slowly added until precipitate
  5. customformed
  6. temperatureThe resulting mixture was cooled in the refrigerator for 45 min
  7. filtrationThe solid was filtered
  8. washwashed with cold hexane
  9. customair-dried

출처 및 근거

ORD 기록
ord-9684e8adf9184acb8cb76ac735974cbb
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217060B2

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