Hydrochloric Acid → HCID 15586694, 화합물

HRID 255699노트

반응식

HRID 255699 반응식
[Cl:1][C:2]1[CH:29]=[CH:28][CH:27]=[CH:26][C:3]=1[C:4]([NH:6][C:7]1[C:8]([N:13]([CH2:20][CH2:21][CH2:22][N:23]([CH3:25])[CH3:24])[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[N:9][CH:10]=[CH:11][CH:12]=1)=O.P(Cl)(Cl)(Cl)=O.Cl>ClC(Cl)C(Cl)Cl>[Cl:1][C:2]1[CH:29]=[CH:28][CH:27]=[CH:26][C:3]=1[C:4]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[N:13]([CH2:20][CH2:21][CH2:22][N:23]([CH3:25])[CH3:24])[C:8]2[N:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 24813Phosphorus oxychlorideHCID 13560178HCID 13560178, 화합물

생성물 1

HCID 15586694HCID 15586694, 화합물

시약·촉매·용매 1

HCID 65911,1,2,2-Tetrachloroethane용매

실험 절차

A solution of 7.0 g (0.017 mole) of 2-chloro-N-[2-[[3-(dimethylamino)propyl]phenylamino]-3-pyridinyl]benzamide and 10.5 g (0.069 mole) of phosphorus oxychloride in 5 ml of 1,1,2,2-tetrachlorethane was heated under nitrogen atmosphere at 110°-115° C. for 16 hr. The cooled reaction mixture was poured into ice and 10 ml of dilute hydrochloric acid added. The mixture was extracted twice with petroleum ether. The acidic portion was made basic with sodium hydroxide pellets and thereafter extracted twice with methylene chloride. The combined methylene chloride extracts were washed with water, dried over sodium sulfate and concentrated in vacuo. The residue was crystallized from isopropyl ether yielding 6.0 g (90%) of material. Recrystallization from isopropyl alcohol-isopropyl ether gave a yellow solid, m.p. 104°-105.6° C.

후처리

  1. customThe cooled reaction mixture
  2. additionadded
  3. extractionThe mixture was extracted twice with petroleum ether
  4. extractionextracted twice with methylene chloride
  5. washThe combined methylene chloride extracts were washed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated in vacuo
  8. customThe residue was crystallized from isopropyl ether yielding 6.0 g (90%) of material
  9. customRecrystallization from isopropyl alcohol-isopropyl ether
  10. customgave a yellow solid, m.p. 104°-105.6° C.

출처 및 근거

ORD 기록
ord-d6b73562585c435797b716cbfe4f3170
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04698430

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