Hydrochloric Acid → N-(4-chloro-3-nitrophenyl)methanesulfonamide

HRID 1493105ノート

反応式

HRID 1493105 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[Cl:6][C:7]1[CH:13]=[CH:12][C:10]([NH2:11])=[CH:9][C:8]=1[N+:14]([O-:16])=[O:15].Cl.O>N1C=CC=CC=1.C1(C)C(C)=CC=CC=1>[Cl:6][C:7]1[CH:13]=[CH:12][C:10]([NH:11][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:9][C:8]=1[N+:14]([O-:16])=[O:15]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 124774-Chloro-3-nitroanilineHCID 31297Methanesulfonyl chloride

生成物 1

HCID 3755760N-(4-chloro-3-nitrophenyl)methanesulfonamide収率 78.1%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 7237O-Xylene溶媒

実験手順

Methanesulphonyl chloride (58.3 g, 0.509 mole) was added in one portion to a stirred solution of 97% 4-chloro-3-nitroaniline (86 g, 0.485 mole) in pyridine (80 ml) and xylene (500 ml). The temperature rose to 50° and the mixture was allowed to stand for a further 2 hr before addition of a mixture of 10M-hydrochloric acid (100 ml) and water (100 ml). The brown solid which was collected and washed successively with xylene (50 ml) and water (3×50 ml). The damp material was crystallized from methanol (800 ml) to give a solid which was collected, washed with methanol (2×50 ml) and dried to give the product 95 g (78%) m.p. 163°.

後処理

  1. customrose to 50°
  2. customThe brown solid which was collected
  3. washwashed successively with xylene (50 ml) and water (3×50 ml)
  4. customThe damp material was crystallized from methanol (800 ml)
  5. customto give a solid which
  6. customwas collected
  7. washwashed with methanol (2×50 ml)
  8. customdried

出典と根拠

ORDレコード
ord-72e351e850fe4f548665b422a5a79849
出典データセット
uspto-grants-1991_06
特許番号
US05021333

反応ノート

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