Methyl iodide → HCID 13686311, 화합물

HRID 1381473노트

반응식

HRID 1381473 반응식
[Cl:1][C:2]1[C:10]2[S:9](=[O:12])(=[O:11])[NH:8][CH2:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[CH3:13]C(C)([O-])C.[K+].CI>CN(C)C=O>[CH3:13][N:8]1[CH2:7][C:6]2[CH:5]=[CH:4][CH:3]=[C:2]([Cl:1])[C:10]=2[S:9]1(=[O:12])=[O:11]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 136863107-Chloro-2,3-dihydrobenzo[d]isothiazole 1,1-DioxideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 13686311HCID 13686311, 화합물수율 86.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 16.6 g of 7-chloro-2,3-dihydro-1,2-benzisothiazole-1,1-dioxide in 85 mls of dry dimethylformamide was cooled and treated with 10 g of potassium t-butoxide at such a rate that the temperature remained below 6° C. The resulting suspension was stirred at 5° to 10° C. for 30 minutes, treated with 6.1 mls of methyl iodide at 10° to 15° C. and stirred at room temperature for 16 hours. The mixture was poured into ice water and the resulting solid was filtered, washed with water and dried in vacuo at 50° C. for 1.5 hours to give 15.4 g of the title compound as a pinkish solid, m.p. 95°-97° C.

후처리

  1. customremained below 6° C
  2. stirringstirred at room temperature for 16 hours
  3. filtrationthe resulting solid was filtered
  4. washwashed with water
  5. customdried in vacuo at 50° C. for 1.5 hours

출처 및 근거

ORD 기록
ord-719b1a0256a6412eb001b9d66a144d2e
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04802911

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