Hydrochloric Acid → HCID 21698798, 화합물

HRID 2395912노트

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HRID 2395912 반응식
Cl.[CH3:2][O:3][C:4]1[C:5]([NH2:10])=[CH:6][CH:7]=[CH:8][CH:9]=1.[N:11]([O-])=O.[Na+].[CH3:15][O:16][CH2:17][CH2:18][CH2:19][NH:20][C:21]1[C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH:24]=[CH:23][CH:22]=1>C1(C)C(C)=CC=CC=1>[CH3:2][O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]=[N:11][C:24]1[C:25]2[C:30](=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:21]([NH:20][CH2:19][CH2:18][CH2:17][O:16][CH3:15])=[CH:22][CH:23]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 70002-Methoxyaniline2회HCID 88339N-(3-Methoxypropyl)naphthalen-1-amineHCID 23668193Sodium Nitrite

생성물 1

HCID 21698798HCID 21698798, 화합물

시약·촉매·용매 1

HCID 7237O-Xylene용매

반응 조건

온도
70 °C

실험 절차

To a three liter flask was charged 200 grams of ice and 1.25 moles of hydrochloric acid. 63.6 grams of o-anisidine was added. At a temperature of 0°-3° C. was added 35 gm of sodium nitrite as a 40% solution. Once the o-anisidine was fully diazotized, 100 gm. of methoxypropyl alpha naphthylamine and 100 gm of xylene were added. The pH was then raised to between 3.5 and 4.0 with a mineral alkaline buffering agent. The coupling temperature was maintained at between 8°-12° C. while the mixture was stirred for 4 hours until a negative coupling test was achieved. The reaction was heated to 70°C. An organic layer was separated from an aqueous phase. Xylene was stripped under vacuum. The non-volatile tarry substance was dissolved in an aromatic high flash solvent which is 50% product/50% viscosity depressant, which solution is stable at -20° C. indefinitely.

후처리

  1. temperatureThe pH was then raised to between 3.5 and 4.0 with a mineral alkaline buffering agent
  2. temperatureThe coupling temperature was maintained at between 8°-12° C. while the mixture
  3. customAn organic layer was separated from an aqueous phase
  4. dissolutionThe non-volatile tarry substance was dissolved in an aromatic high flash solvent which
  5. customis stable at -20° C.

출처 및 근거

ORD 기록
ord-fdf3c3b54a0e4017976f3beb5a4eb99d
출처 데이터셋
uspto-grants-1996_02
특허 번호
US05490872

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