تفاعل #1162802

ord-51aa7c0bd8c94e34936dc0a39f0005f5

معادلة التفاعل

[Na+].[O-][Cl+3]([O-])([O-])[O-]
sodium perchlorate
CC1(C)CCC(C)(C)c2cc(O)ccc21
5,5,8,8-tetramethyl-5,6,7,8tetrahydronaphthalen-2-ol
[Na+].[OH-]
sodium hydroxide
[I-].[Na+]
sodium iodide
Cl
hydrochloric acid
O=S([O-])([O-])=S.[Na+].[Na+]
sodium thiosulfate
CC1(C)CCC(C)(C)c2cc(I)c(O)cc21
3-iodo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ol

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was maintained
  2. 2
    workup.STIRRINGAfter stirring
  3. 3
    استخلاصIt was extracted with 200 ml of ethyl ether
  4. 4
    غسيلThe organic phase was washed twice with 400 ml of water
  5. 5
    تجفيفdried over magnesium sulfate
  6. 6
    تركيزconcentrated in a rotary evaporator under vacuum at 40° C.

الإجراء التجريبي

A 3.6% sodium perchlorate solution was added dropwise to a mixture of 5,5,8,8-tetramethyl-5,6,7,8tetrahydronaphthalen-2-ol(6.35 g, 31.1 mmol), sodium hydroxide (1.23 g, 34.2 mmol) and sodium iodide (4.6 g, 31.1 mmol) in methanol (115 ml), at 0° C. The mixture was maintained under stirring for two hours at 0° C. 33 ml of a 10% sodium thiosulfate solution were added. After stirring, the mixture was acidified with hydrochloric acid to pH 1. It was extracted with 200 ml of ethyl ether. The organic phase was washed twice with 400 ml of water, dried over magnesium sulfate and concentrated in a rotary evaporator under vacuum at 40° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05905088uspto-grants-1999_05