Hydrochloric Acid → HCID 178499608, 화합물

HRID 44217

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HRID 44217 반응식
Cl.[N+:2]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C:12](=[NH:14])[NH2:13])=[CH:7][CH:6]=1)([O-:4])=[O:3].[CH:15]([C:27](OCC)=[O:28])([C:22](OCC)=[O:23])[CH2:16][C:17]([O:19][CH2:20]C)=[O:18].C[O-].[Na+].Cl>O.CO>[OH:23][C:22]1[C:15]([CH2:16][C:17]([O:19][CH3:20])=[O:18])=[C:27]([OH:28])[N:13]=[C:12]([CH2:11][C:8]2[CH:7]=[CH:6][C:5]([N+:2]([O-:4])=[O:3])=[CH:10][CH:9]=2)[N:14]=1

참가 물질

7

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HCID 313Hydrochloric AcidHCID 81961Triethyl ethane-1,1,2-tricarboxylateHCID 10942334Sodium MethoxideHCID 463184212-(4-Nitrophenyl)ethanimidamide hydrochloride

생성물 1

HCID 178499608HCID 178499608, 화합물

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 962Water용매

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온도
0 °C

실험 절차

A 250 mL round bottom flask was charged with 2-(4-nitrophenyl)ethanimidamide hydrochloride (approximately 6.47 g, 30.0 mmol, 48% purity), triethyl ethane-1,1,2-tricarboxylate (7.60 mL, 33.0 mmol) and methanol (43 mL). To this solution was added a 25% sodium methoxide solution in methanol (24.0 mL, 105.2 mmol) immediately resulting in a dark purple thick suspension. After stirring for three hours under reflux the dark purple mixture was cooled to 0° C. using an ice bath and carefully treated with 30 mL water. This mixture was slowly treated with 35 mL 6N hydrochloric acid giving a pale green suspension. The suspension was stirred for additional 30 minutes, filtered and the obtained fawn solid was washed with 100 mL water. The product was dried in a desiccator under vacuum for two days. The crude product was used without purification in the next step.

후처리

  1. customimmediately resulting in a dark purple thick suspension
  2. temperatureunder reflux the dark purple mixture
  3. stirringThe suspension was stirred for additional 30 minutes
  4. filtrationfiltered
  5. washthe obtained fawn solid was washed with 100 mL water
  6. customThe product was dried in a desiccator under vacuum for two days
  7. customThe crude product was used without purification in the next step

출처 및 근거

ORD 기록
ord-896753e013a64ab8ab5ba568d4ebf1c3
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541419B2

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