Hydroxyamine hydrochloride → HCID 178513239, 화합물

HRID 1512740노트

반응식

HRID 1512740 반응식
Cl.[NH2:2][OH:3].C(=O)(O)[O-].[Na+].[OH:9][CH2:10][C:11]1[NH:12][C:13]2[C:18]([CH:19]=1)=[CH:17][C:16]([C:20]#[N:21])=[CH:15][CH:14]=2>CCO>[OH:3][NH:2][C:20]([C:16]1[CH:17]=[C:18]2[C:13](=[CH:14][CH:15]=1)[NH:12][C:11]([CH2:10][OH:9])=[CH:19]2)=[NH:21]

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochloride2회HCID 516892Sodium Bicarbonate2회HCID 135679562-(hydroxymethyl)-1H-indole-5-carbonitrile

생성물 1

HCID 178513239HCID 178513239, 화합물수율 83.9%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
50 °C

실험 절차

Hydroxylamine hydrochloride (243 mg) and sodium bicarbonate (586 mg) was added to a solution of 2-(hydroxymethyl)-1H-indole-5-carbonitrile (D24) (300 mg) in EtOH (20 mL), in that sequence. The reaction mixture was heated to 50° C. and stirred for 24 hours at that temperature. Another portion of hydroxylamine hydrochloride (100 mg) was added, followed by addition of sodium bicarbonate (220 mg). The resulting suspension was stirred at 50° C. for 7 hours. The inorganics was filtered off. The filtrate was concentrated to afford a pale yellow oil. Trituration of the residue provided N-hydroxy-2-(hydroxymethyl)-1H-indole-5-carboximidamide (D25) (300 mg) as a pale yellow solid. MS (ES): C10H11N3O2 requires 205; found 206.2 (M+H+).

후처리

  1. stirringThe resulting suspension was stirred at 50° C. for 7 hours
  2. filtrationThe inorganics was filtered off
  3. concentrationThe filtrate was concentrated
  4. customto afford a pale yellow oil

출처 및 근거

ORD 기록
ord-5a5292c9195e4e6886e8769c03960f97
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217028B2

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