2-Chloroethanol → Phenol, 4-[(2-chloroethyl)thio]-

HRID 845089ノート

反応式

HRID 845089 の反応式
[Cl:1][CH2:2]CO.[OH:5][C:6]1[CH:11]=[CH:10][C:9]([S:12][C:13]#N)=[CH:8][CH:7]=1.C(P(CC)CC)C>CC(C)=O.O.C(OCC)C>[Cl:1][CH2:2][CH2:13][S:12][C:9]1[CH:10]=[CH:11][C:6]([OH:5])=[CH:7][CH:8]=1

参加物

7

反応物 3

HCID 342-ChloroethanolHCID 27365TriethylphosphineHCID 2203274-Hydroxyphenyl thiocyanate

生成物 1

HCID 13576289Phenol, 4-[(2-chloroethyl)thio]-

試薬・触媒・溶媒 3

HCID 180Acetone溶媒HCID 962Water溶媒2 回HCID 3283Diethyl Ether溶媒

実験手順

2-chloro-ethanol (3.9 g, 0.049 mole) was added to a solution of the product of Example 35 (7.4 g, 0.049 mole) in water (0.1 mole) and acetone (50 ml). After cooling with an ice bath triethylphosphine (5.6 g, 0.047 mole) was added dropwise over 25 minutes. Ethyl ether (200 ml) and water (75 ml) were added and the layers separated. The organic layer was washed with water (4×50 ml) and saturated sodium chloride (2×25 ml) dried over magnesium sulfate, filtered and concentrated to give a yellow oil. The structure was confirmed by its NMR spectrum.

後処理

  1. additionwas added dropwise over 25 minutes
  2. customthe layers separated
  3. washThe organic layer was washed with water (4×50 ml) and saturated sodium chloride (2×25 ml)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto give a yellow oil

出典と根拠

ORDレコード
ord-3709ffa22d0d4450bea236aa4ebfb0cf
出典データセット
uspto-grants-1988_07
特許番号
US04755524

反応ノート

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