Dichloromethane → HCID 20197936、化合物

HRID 1731784

反応式

HRID 1731784 の反応式
Cl[S:2][N:3]([CH3:7])[C:4](=[O:6])[O-:5].[Cl:8][C:9]1[CH:22]=[C:21]([C:23]([F:26])([F:25])[F:24])[CH:20]=[CH:19][C:10]=1[O:11][C:12]1[CH:18]=[CH:17][C:15]([NH2:16])=[CH:14][CH:13]=1.C(N([CH2:32][CH3:33])CC)C.[CH2:34](Cl)Cl>>[Cl:8][C:9]1[CH:22]=[C:21]([C:23]([F:25])([F:24])[F:26])[CH:20]=[CH:19][C:10]=1[O:11][C:12]1[CH:13]=[CH:14][C:15]([NH:16][S:2][N:3]([CH3:7])[C:4](=[O:6])[O:5][CH2:34][CH2:32][CH3:33])=[CH:17][CH:18]=1

参加物

5

反応物 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 104693274-[2-Chloro-4-(trifluoromethyl)phenoxy]anilineHCID 131714972N-chlorosulphenyl-N-methylcarbamate

生成物 1

HCID 20197936HCID 20197936、化合物

実験手順

A solution of 3.7 g of N-chlorosulphenyl-N-methylcarbamate in 10 ml of dry methylene chloride was added over 20 minutes to a stirred solution of 6.3 g of 4-[2-chloro-4-(trifluoromethyl)phenoxy]aniline in 25 ml of the same solvent containing 2.5 g of triethylamine. The reaction mixture temperature was kept at 0°-5° C. by means of an ice bath until the addition was completed, and was then allowed to rise to ambient temperature over 2.0 hours. The solvent was removed under reduced pressure and the residue was suspended in 200 ml of diethyl ether and washed three times with water. The resulting ether solution was dried (MgSO4) and the solvent was evaporated. The residue was purified by rapid chromatography on silica gel using methylene chloride as eluent. Crystallisation from diethyl ether/light petroleum gave 1, as pale buff-coloured crystals (m.p.: 61°-64° C.).

後処理

  1. additionThe reaction mixture temperature was kept at 0°-5° C. by means of an ice bath until the addition
  2. customThe solvent was removed under reduced pressure
  3. washwashed three times with water
  4. dry with materialThe resulting ether solution was dried (MgSO4)
  5. customthe solvent was evaporated
  6. customThe residue was purified by rapid chromatography on silica gel
  7. customCrystallisation from diethyl ether/light petroleum
  8. customgave 1

出典と根拠

ORDレコード
ord-a438f86bf0424e7c90a5df88d40423af
出典データセット
uspto-grants-1986_11
特許番号
US04623658

関連ノート

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