Hydrochloric Acid → p-Phenylene benzobisoxazole

HRID 2419532ノート

反応式

HRID 2419532 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[OH:8].Cl[C:10](Cl)(Cl)[C:11]1[CH:19]=[CH:18][C:14]([C:15](Cl)=[O:16])=[CH:13][CH:12]=1.Cl>>[C:14]1([C:15]2[O:16][C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[N:1]=2)[CH:18]=[CH:19][C:11]([C:10]2[O:8][C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[N:1]=2)=[CH:12][CH:13]=1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 58012-AminophenolHCID 846604-(Trichloromethyl)benzoyl chloride

生成物 1

HCID 691763p-Phenylene benzobisoxazole収率 71.4%

実験手順

In the apparatus described under Example 1, 21.8 g of reactant A (0.2 mol), 25.8 g of p-trichloromethyl-benzoyl chloride (0.1 mol) and 3.5 g of B2O3 (0.05 mol) were mixed and slowly heated. Between 190° and 200° C, a vigorous evolution of HCl began. After 2 hours the mixture was cooled and ground in a mortar. After extraction twice with 100 ml of CHCl3 and twice with 100 ml of water, 22.3 g of raw product (71% of the theory) was obtained, melting at 318° to 328° C. Compound XIX can be recrystallized from dimethylformamide, o-dichlorobenzene, nitrobenzene, dimethylsulfoxide or 1,2-dibromoethane. A small specimen recrystallized from o-dichlorobenzene melted at 325° to 329° C. The product can be further purified by chromatography on Al2O3 with 1,2-dibromoethane as the elutant at 120° C, whereupon the melting point becomes 340° to 342° C.

後処理

  1. additionwere mixed
  2. temperatureslowly heated
  3. customBetween 190°
  4. custom200° C
  5. temperatureAfter 2 hours the mixture was cooled
  6. extractionAfter extraction twice with 100 ml of CHCl3

出典と根拠

ORDレコード
ord-0774dcbcc53047bd9bd8442e5bfceeee
出典データセット
uspto-grants-1978_08
特許番号
US04107169

反応ノート

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