Hydrochloric Acid → HCID 40787308、化合物

HRID 1091901ノート

反応式

HRID 1091901 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[NH2:9].N1C=CC=CC=1.[F:16][C:17]([F:29])([F:28])[C:18]1[CH:23]=[CH:22][C:21]([S:24](Cl)(=[O:26])=[O:25])=[CH:20][CH:19]=1.Cl>ClCCl.C(OCC)C>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[NH:9][S:24]([C:21]1[CH:20]=[CH:19][C:18]([C:17]([F:16])([F:28])[F:29])=[CH:23][CH:22]=1)(=[O:26])=[O:25]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 97092,4-DifluoroanilineHCID 27773994-(Trifluoromethyl)benzenesulfonyl chloride

生成物 1

HCID 40787308HCID 40787308、化合物収率 34.6%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

To 2,4-difluoro-phenylamine (1, 2.09 mL, 20.7 mmol) in 13.04 mL of dichloromethane, pyridine (0.522 mL, 6.45 mmol) was added and the mixture was stirred under nitrogen for 20 minutes. 4-Trifluoromethyl-benzenesulfonyl chloride (2, 5.00 g, 20.4 mmol) was added slowly and the reaction was stirred overnight. The reaction mixture was treated with 2 mL of 1 M hydrochloric acid in diethyl ether and allowed to sit for 1 hour. The solid precipitate was filtered off, and the filtrate was extracted with 1 N aqueous hydrochloric acid followed by brine. The organic portion was dried over magnesium sulfate, filtered and the filtrate was concentrated under vacuum. The resulting solid was treated with dichloromethane, and the solid was collected and dried to provide the desired compound as a white solid (3, 2.383 g).

後処理

  1. stirringthe reaction was stirred overnight
  2. waitto sit for 1 hour
  3. filtrationThe solid precipitate was filtered off
  4. extractionthe filtrate was extracted with 1 N aqueous hydrochloric acid
  5. dry with materialThe organic portion was dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated under vacuum
  8. additionThe resulting solid was treated with dichloromethane
  9. customthe solid was collected
  10. customdried

出典と根拠

ORDレコード
ord-b60114c823324ef28cdc2e160449991d
出典データセット
uspto-grants-2012_03
特許番号
US08129404B2

反応ノート

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