Triethylamine → (E)-1-Chloro-4-(2-tosylvinyl)benzene

HRID 623722ノート

反応式

HRID 623722 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8](I)[CH2:9][S:10]([C:13]2[CH:19]=[CH:18][C:16]([CH3:17])=[CH:15][CH:14]=2)(=[O:12])=[O:11])=[CH:4][CH:3]=1.CCN(CC)CC>CC#N>[Cl:1][C:2]1[CH:7]=[CH:6][C:5](/[CH:8]=[CH:9]/[S:10]([C:13]2[CH:14]=[CH:15][C:16]([CH3:17])=[CH:18][CH:19]=2)(=[O:11])=[O:12])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 8471TriethylamineHCID 86711813HCID 86711813、化合物

生成物 1

HCID 10979228(E)-1-Chloro-4-(2-tosylvinyl)benzene収率 96%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

1-Chloro-4-(1-iodo-2-tosylethyl)benzene (28.5 g, 67.7 mmol) was dissolved in dry MeCN (376 mL) followed by addition of Et3N (18.83 mL, 135 mmol) and the mixture was stirred at room temperature for 1 h. Then the solvent was evaporated under reduced pressure and the residue partitioned between DCM (400 mL) and 1M aqueous KHSO4 (300 mL). The layers were separated and the organic phase was dried over Na2SO4, filtered and evaporated to dryness under reduced pressure to afford 19 g (96%) of the desired product.

後処理

  1. customThen the solvent was evaporated under reduced pressure
  2. customthe residue partitioned between DCM (400 mL) and 1M aqueous KHSO4 (300 mL)
  3. customThe layers were separated
  4. dry with materialthe organic phase was dried over Na2SO4
  5. filtrationfiltered
  6. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-54e42c48060c417fb8cb1a0a23734422
出典データセット
uspto-grants-2016_04
特許番号
US09302988B2

反応ノート

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