Hydroxyamine hydrochloride → 1H-indole-7-carbaldehyde oxime

HRID 1512722노트

반응식

HRID 1512722 반응식
Cl.[NH2:2][OH:3].[NH:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[CH:13]=O)[CH:6]=[CH:5]1>N1C=CC=CC=1>[NH:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[CH:13]=[N:2][OH:3])[CH:6]=[CH:5]1

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 2734629Indole-7-carboxaldehyde

생성물 1

HCID 734136671H-indole-7-carbaldehyde oxime

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Hydroxylamine hydrochloride (0.574 g) was added portionwise to a solution of 1H-indole-7-carbaldehyde (1 g) in pyridine (5 ml) at RT. The resulting solution was heated to reflux and kept at that temperature for 1 hour. The solvent was evaporated. Ethyl acetate (50 mL) was added and the resulting solution was washed with aqueous hydrochloric acid (0.5 M, 40 mL). The organic fraction was separated and dried over anhydrous magnesium sulfate. The dried solution was concentrated to afford 1H-indole-7-carbaldehyde oxime (D1) as a colorless oil which, upon standing, solidified to give a waxy solid (1.1 g). MS (ES): C9H8N2O requires 160; found 161.1 (M+H+).

후처리

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux
  3. customThe solvent was evaporated
  4. additionEthyl acetate (50 mL) was added
  5. washthe resulting solution was washed with aqueous hydrochloric acid (0.5 M, 40 mL)
  6. customThe organic fraction was separated
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationThe dried solution was concentrated

출처 및 근거

ORD 기록
ord-5a548ac4f3c84a0a8fbe60225ab04f3a
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217028B2

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