Phosphorus pentachloride → HCID 54565141、化合物

HRID 66209ノート

反応式

HRID 66209 の反応式
[N+:1]([C:4]1[CH:23]=[CH:22][C:7]([CH:8]=[CH:9][S:10]([NH:13][C:14](=O)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)(=[O:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].P(Cl)(Cl)(Cl)(Cl)[Cl:25]>C1C=CC=CC=1>[N+:1]([C:4]1[CH:23]=[CH:22][C:7]([CH:8]=[CH:9][S:10]([N:13]=[C:14]([Cl:25])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)(=[O:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

4

反応物 2

HCID 24819Phosphorus pentachlorideHCID 54406439N-(4-nitrostyrylsulfonyl)benzamide

生成物 1

HCID 54565141HCID 54565141、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A suspension of N-(4-nitrostyrylsulfonyl)benzamide (14.9 g., 0.045 mole) in 500 ml. of dry benzene is refluxed and stirred with phosphorus pentachloride (10.4 g., 0.05 mole) for 8 hr. The reaction mixture after standing overnight at 25° C. provides 8.2 g. of solid, m.p. 158°-166° C. Concentration of the mother liquor to about 100 ml. provides an additional 2.5 g. of solid, m.p. 158°-161° C. The combined crude solid crystallized from ethyl acetate affords analytically pure N-(4-nitrostyrylsulfonyl)benzimidoyl chloride, m.p. 168°-175° C.

後処理

  1. customprovides 8.2 g
  2. customprovides an additional 2.5 g
  3. customcrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-1ff354add50842419cca2a7e164ab251
出典データセット
uspto-grants-1978_12
特許番号
US04130663

反応ノート

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