Water → HCID 178458783, 화합물

HRID 2236540노트

반응식

HRID 2236540 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178458783HCID 178458783, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-04458ab4061e476fa4970e21fc5eca61
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713994B2

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