Hydrochloric Acid → HCID 15586694、化合物

HRID 255699ノート

反応式

HRID 255699 の反応式
[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

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24813Phosphorus oxychlorideHCID 13560178HCID 13560178、化合物

生成物 1

HCID 15586694HCID 15586694、化合物

試薬・触媒・溶媒 1

HCID 65911,1,2,2-Tetrachloroethane溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-d6b73562585c435797b716cbfe4f3170
出典データセット
uspto-grants-1987_10
特許番号
US04698430

反応ノート

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