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

HRID 986306노트

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HRID 986306 반응식
[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.C(OCC)C>CC(C)=O.O>[Cl:1][CH2:2][CH2:13][S:12][C:9]1[CH:10]=[CH:11][C:6]([OH:5])=[CH:7][CH:8]=1

참가 물질

7

반응물 4

HCID 342-ChloroethanolHCID 3283Diethyl EtherHCID 27365TriethylphosphineHCID 2203274-Hydroxyphenyl thiocyanate

생성물 1

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

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

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 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.

후처리

  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

출처 및 근거

ORD 기록
ord-71344744096c43ee9e45e883f849716f
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04711903

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