Water → HCID 178458783、化合物

HRID 2236540ノート

反応式

HRID 2236540 の反応式
[N:1]([CH2:4][C:5]1[CH:10]=[C:9]([OH:11])[C:8]([O:12][CH2:13][CH2:14][CH3:15])=[CH:7][N:6]=1)=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O>O1CCCC1>[NH2:1][CH2:4][C:5]1[CH:10]=[C:9]([OH:11])[C:8]([O:12][CH2:13][CH2:14][CH3:15])=[CH:7][N:6]=1

参加物

5

反応物 3

HCID 962WaterHCID 11776TriphenylphosphineHCID 1784587892-Azidomethyl-5-propoxy-pyridin-4-ol

生成物 1

HCID 178458783HCID 178458783、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 2-azidomethyl-5-propoxy-pyridin-4-ol (9.70 g, 46.6 mole), is then suspended in 120 mL of tetrahydrofuran and treated with triphenylphosphine (12.22 g, 46.6 mmole) after stirring for 10 mins at ambient temperature water is added (12.6 mL, 15 equivalents) and the reaction mixture is stirred at ambient temperature overnight. The solids gradually dissolved followed by the formation of a precipitate. The resulting solid is filtered, washed with fresh 10:1 tetrahydrofuran:water and dried to give, 5.92 g, (69%), mp 159-60° C.; MS (ES+): m/z 183.3 (M+H).

後処理

  1. additionis added (12.6 mL, 15 equivalents)
  2. dissolutionThe solids gradually dissolved
  3. filtrationThe resulting solid is filtered
  4. washwashed with fresh 10:1 tetrahydrofuran
  5. dry with materialwater and dried
  6. customto give

出典と根拠

ORDレコード
ord-04458ab4061e476fa4970e21fc5eca61
出典データセット
uspto-grants-2010_05
特許番号
US07713994B2

反応ノート

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