Water → [5-(2,6-Dichloro-4-trifluoromethylphenyl)-2-methylphenyl]isopropyl sulfide

HRID 1823153ノート

反応式

HRID 1823153 の反応式
[S:1]([C:21]1[CH:26]=C(C2C(Cl)=CC(C(F)(F)F)=CC=2Cl)C=C[C:22]=1C)[C:2]1[CH:7]=[C:6]([C:8]2[C:13]([Cl:14])=[CH:12][C:11]([C:15]([F:18])([F:17])[F:16])=[CH:10][C:9]=2[Cl:19])[CH:5]=[CH:4][C:3]=1[CH3:20].C(S([O-])=O)O.[Na+].C(I)(C)C.O>CN(C)C=O>[Cl:19][C:9]1[CH:10]=[C:11]([C:15]([F:17])([F:18])[F:16])[CH:12]=[C:13]([Cl:14])[C:8]=1[C:6]1[CH:5]=[CH:4][C:3]([CH3:20])=[C:2]([S:1][CH:21]([CH3:22])[CH3:26])[CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 6362Isopropyl iodideHCID 221709441,1'-Thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene]HCID 23689980Sodium Formaldehyde Sulfoxylate

生成物 1

HCID 12137642[5-(2,6-Dichloro-4-trifluoromethylphenyl)-2-methylphenyl]isopropyl sulfide収率 75.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3.3 g (4.9 mmol) of 1,1′-thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene], 3,0 g (19.5 mmol) of Rongalite and 3.0 g (17.6 mmol) of isopropyl iodide were stirred in 30 ml of N,N-dimethylformamide at room temperature for 3 hours. The resulting reaction mixture was poured into 300 ml of water and extracted with 50 ml of ethyl acetate twice. The ethyl acetate layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 1.4 g of [5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylphenyl]isopropyl sulfide (yield 38.0%) as a yellow dough (nD20 1.5462).

後処理

  1. customThe resulting reaction mixture
  2. extractionextracted with 50 ml of ethyl acetate twice
  3. washThe ethyl acetate layer was washed with 50 ml of water twice
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe ethyl acetate was distilled off under reduced pressure
  6. customPurification of the residue by silica gel column chromatography

出典と根拠

ORDレコード
ord-d5c22e8c887b4258ad617601832819bb
出典データセット
uspto-grants-2006_05
特許番号
US07037930B2

反応ノート

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