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Hydrochloric Acid → 1-Trityl-1H-imidazole-4-carboxylic acid

HRID 2063271
ノート
印刷プレビュー

反応式

HRID 2063271 の反応式
C[O:2][C:3]([C:5]1[NH:6][CH:7]=[N:8][CH:9]=1)=[O:4].C(N(CC)CC)C.Cl[C:18]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[OH-].[Li+].Cl>C(Cl)Cl.O>[C:18]([N:8]1[CH:9]=[C:5]([C:3]([OH:2])=[O:4])[N:6]=[CH:7]1)([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)([C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1)[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 6456Trityl chlorideHCID 8471TriethylamineHCID 565661Methyl 1H-imidazole-5-carboxylate

生成物 1

HCID 105701171-Trityl-1H-imidazole-4-carboxylic acid

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒2 回

実験手順

3H-Imidazole-4-carboxylic acid methyl ester (9.86 g, 78.2 mmol) is taken up in 150 mL DCM, triethylamine (11.9 mL, 86.0 mmol) is added and the reaction mixture is stirred for 5 min at RT. Chlorotriphenylmethane (24.0 g, 86.0 mmol) is added and the reaction mixture is stirred overnight at RT. The reaction mixture is extracted with an aqueous 5% NaHCO3 solution, the organic phase is dried over MgSO4 and concentrated under reduced pressure. The residue (20.7 g) is taken up in 100 mL MeOH, a solution of lithium hydroxide (4.80 g, 24.0 mmol) in 20 mL water is added drop wise and the reaction mixture is stirred over weekend at RT. The reaction mixture is acidified to pH 4 with 6N hydrochloric acid, 200 mL DCM is added and the two phase mixture is stirred vigorously. The phases are separated and the organic phase is dried over MgSO4 and concentrated under reduced pressure. Yield: 19.2 g. HPLC-MS: double peak tR=2.55/2.67 min, (M−H)−=353.

後処理

  1. stirringthe reaction mixture is stirred overnight at RT
  2. extractionThe reaction mixture is extracted with an aqueous 5% NaHCO3 solution
  3. dry with materialthe organic phase is dried over MgSO4
  4. concentrationconcentrated under reduced pressure
  5. stirringthe reaction mixture is stirred over weekend at RT
  6. additionis added
  7. stirringthe two phase mixture is stirred vigorously
  8. customThe phases are separated
  9. dry with materialthe organic phase is dried over MgSO4
  10. concentrationconcentrated under reduced pressure
  11. custom2.67 min, (M−H)−=353

出典と根拠

ORDレコード
ord-ae7d40e5f3a74283aa13cd17a97c1e6b
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08288379B2

反応ノート

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