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Hydrochloric Acid → HCID 178423463, 화합물

HRID 1842488
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HRID 1842488 반응식
[CH3:1][C:2]1[CH:21]=[CH:20][C:5]2[NH:6][C:7]([CH:9]3[CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10]3)=[N:8][C:4]=2[CH:3]=1.[ClH:22]>O1CCOCC1>[ClH:22].[ClH:22].[NH:11]1[CH2:12][CH:9]([C:7]2[NH:6][C:5]3[CH:20]=[CH:21][C:2]([CH3:1])=[CH:3][C:4]=3[N:8]=2)[CH2:10]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 178423469HCID 178423469, 화합물

생성물 1

HCID 178423463HCID 178423463, 화합물수율 84%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To tert-butyl 3-(5-methyl-1H-benzo[d]imidazol-2-yl)azetidine-1-carboxylate (prepared in the previous step) was added 4 M HCl in dioxane (30 mL). The reaction mixture was stirred at RT. After 30 min, a solid coated the inside of the flask. The liquid was removed from the flask and the remaining solid was dried under high vacuum. The solid was dissolved in MeOH (20 mL) and diluted with ether (50 mL). The precipitate was collected by filtration and dried under high vacuum to give 2-(azetidin-3-yl)-5-methyl-1H-benzo[d]imidazole dihydrochloride (2.99 g, 11.5 mmol 84% yield over three steps) as a dark red solid.

후처리

  1. customThe liquid was removed from the flask
  2. customthe remaining solid was dried under high vacuum
  3. dissolutionThe solid was dissolved in MeOH (20 mL)
  4. additiondiluted with ether (50 mL)
  5. filtrationThe precipitate was collected by filtration
  6. customdried under high vacuum

출처 및 근거

ORD 기록
ord-3d6aaac42ba24692be9c8ed865f5f89e
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946230B2

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