Hydrochloric Acid → HCID 21698798、化合物

HRID 2395912ノート

反応式

HRID 2395912 の反応式
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

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 70002-Methoxyaniline2 回HCID 88339N-(3-Methoxypropyl)naphthalen-1-amineHCID 23668193Sodium Nitrite

生成物 1

HCID 21698798HCID 21698798、化合物

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-fdf3c3b54a0e4017976f3beb5a4eb99d
出典データセット
uspto-grants-1996_02
特許番号
US05490872

反応ノート

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