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Chloroform → HCID 12223711, 화합물

HRID 1658057
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HRID 1658057 반응식
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:16]=[C:15]2[C:6]([S:7][C:8]3[CH:9]=[CH:10][CH:11]=[C:12]([C:17](O)=[O:18])[C:13]=3[NH:14]2)=[CH:5][CH:4]=1.C(Cl)(Cl)[Cl:23].P(Cl)(Cl)Cl>CN(C)C=O>[F:1][C:2]([F:21])([F:20])[C:3]1[CH:16]=[C:15]2[C:6]([S:7][C:8]3[CH:9]=[CH:10][CH:11]=[C:12]([C:17]([Cl:23])=[O:18])[C:13]=3[NH:14]2)=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6212ChloroformHCID 23647FlutiazinHCID 24387Phosphorus trichloride

생성물 1

HCID 12223711HCID 12223711, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

8-Trifluoromethylphenothiazine-1-carboxylic acid (62.2 g., 0.20 mol.) was added to a stirred mixture of 300 ml. of chloroform and 300 ml. of phosphorus trichloride. The resulting brown suspension was cooled in an ice-bath while 50 ml. of dimethylformamide was added slowly until a reddish brown solution formed. After stirring the mixture for 4 hours at 25°, the chloroform and excess phosphorus trichloride were evaporated under reduced pressure. The resulting reddish brown solid residue was dissolved in 1500 ml. of boiling n-hexane. The hot, clear, reddish solution was decanted from a viscous, insoluble material and, on cooling, large red needles formed. The solid was collected by filtration and washed with hexane to give 8-trifluoromethylphenothiazine-1-carboxylic acid chloride, m.p. 124°-126°.

후처리

  1. temperatureThe resulting brown suspension was cooled in an ice-bath while 50 ml
  2. customformed
  3. customthe chloroform and excess phosphorus trichloride were evaporated under reduced pressure
  4. dissolutionThe resulting reddish brown solid residue was dissolved in 1500 ml
  5. customThe hot, clear, reddish solution was decanted from a viscous, insoluble material
  6. temperatureon cooling
  7. customlarge red needles formed
  8. filtrationThe solid was collected by filtration
  9. washwashed with hexane

출처 및 근거

ORD 기록
ord-516d230704054dec93bc61421a63a35b
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03962438

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