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Hydrochloric Acid → HCID 178423463、化合物

HRID 1842488
ノート
印刷プレビュー

反応式

HRID 1842488 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 178423469HCID 178423469、化合物

生成物 1

HCID 178423463HCID 178423463、化合物収率 84%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3d6aaac42ba24692be9c8ed865f5f89e
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946230B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート