Triphenylphosphine → 5-Chloro-2-methoxybenzene-1-thiol

HRID 1675590ノート

反応式

HRID 1675590 の反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cl:20][C:21]1[CH:22]=[CH:23][C:24]([O:31][CH3:32])=[C:25]([S:27](Cl)(=O)=O)[CH:26]=1>C1COCC1.O>[Cl:20][C:21]1[CH:22]=[CH:23][C:24]([O:31][CH3:32])=[C:25]([SH:27])[CH:26]=1

参加物

5

反応物 2

HCID 11776TriphenylphosphineHCID 27342725-Chloro-2-methoxybenzene-1-sulfonyl chloride

生成物 1

HCID 127727855-Chloro-2-methoxybenzene-1-thiol

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

Triphenylphosphine (11.4 g) was added portionwise to a stirred solution of 5-chloro-2-methoxybenzenesulphonyl chloride (3.0 g) in THF (30 ml). Water (4 ml) was added and the mixture stirred at RT for 2 h, after which the reaction was diluted with water (25 ml) then 2M sodium hydroxide solution and washed with ether. The aqueous layer was acidified with 2M hydrochloric acid and extracted with ethylacetate. The organic layer was dried and evaporated under reduced pressure, yield 3.1 g.

後処理

  1. wash2M sodium hydroxide solution and washed with ether
  2. extractionextracted with ethylacetate
  3. customThe organic layer was dried
  4. customevaporated under reduced pressure, yield 3.1 g

出典と根拠

ORDレコード
ord-c802e92cd8f549e28bc7519933a6f9ba
出典データセット
uspto-grants-2011_08
特許番号
US08003703B2

反応ノート

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