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Hydroxyamine hydrochloride → HCID 54400138, 화합물

HRID 1089583
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HRID 1089583 반응식
C[O-].[Na+].[ClH:4].[NH2:5][OH:6].Cl[C:8]1[CH:17]=[CH:16][CH:15]=[C:14]2[C:9]=1[CH:10]=[CH:11][CH:12]=[C:13]2[CH2:18][C:19]#[N:20]>CO>[OH:6][N:5]=[C:19]([NH2:20])[CH2:18][C:13]1[C:14]2[C:9](=[C:8]([Cl:4])[CH:17]=[CH:16][CH:15]=2)[CH:10]=[CH:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochloride2회HCID 10942334Sodium Methoxide2회HCID 70357837HCID 70357837, 화합물

생성물 1

HCID 54400138HCID 54400138, 화합물수율 69%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A mixture of NaOMe (25 wt % in MeOH, 1.02 mL, 4.46 mmol), MeOH (4 mL), and hydroxylamine hydrochloride (310 mg, 4.46 mmol) was heated at reflux for 20 minutes. 5-Chloro-2-naphthalenylacetonitrile (600 mg, 2.98 mmol) and additional MeOH (4 mL) were added and heating was continued overnight. Additional hydroxylamine hydrochloride (150 mg, 2.16 mmol) and NaOMe (25 wt % in MeOH, 490 μL, 2.14 mmol) were added and heating was resumed for 4 hours. The mixture was cooled, concentrated, and suspended in H2O. The solid was collected by filtration and triturated with ether to give a pale yellow solid (478 mg, 69%), m.p. 121°-125° C.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 20 minutes
  3. temperatureheating
  4. temperatureheating
  5. waitwas resumed for 4 hours
  6. temperatureThe mixture was cooled
  7. concentrationconcentrated
  8. filtrationThe solid was collected by filtration
  9. customtriturated with ether

출처 및 근거

ORD 기록
ord-df6559c25fc44ae79cacdac207a7586a
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04966975

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