홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Methyl iodide → 6-[4-(3,4-Dichloro-phenylsulfinyl)-butoxy]-1,4,4-trimethyl-4H-3,1-benzoxazin-2-one

HRID 463078
노트
인쇄 미리보기

반응식

HRID 463078 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([CH2:11][CH2:12][CH2:13][CH2:14][O:15][C:16]2[CH:17]=[CH:18][C:19]3[NH:24][C:23](=[O:25])[O:22][C:21]([CH3:27])([CH3:26])[C:20]=3[CH:28]=2)=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8].[CH3:29]I.[OH-].[Na+]>C(Cl)Cl.S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC>[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([CH2:11][CH2:12][CH2:13][CH2:14][O:15][C:16]2[CH:17]=[CH:18][C:19]3[N:24]([CH3:29])[C:23](=[O:25])[O:22][C:21]([CH3:26])([CH3:27])[C:20]=3[CH:28]=2)=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 132539416-[4-(3,4-Dichloro-phenylsulfinyl)-butoxy]-4,4-dimethyl-4H-3,1-benzoxazin-2-one

생성물 1

HCID 132540206-[4-(3,4-Dichloro-phenylsulfinyl)-butoxy]-1,4,4-trimethyl-4H-3,1-benzoxazin-2-one

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매
HCID 6344
Dichloromethane
용매

실험 절차

A solution of 1.1 gm (0.0025 mol) of 6-[4-(3,4-dichloro-phenylsulfinyl)-butoxy]-4,4-dimethyl-4H-3,1-benzoxazin-2-one and 1 ml of methyl iodide in 30 ml of methylene chloride are mixed with 30 ml of 2N sodium hydroxide solution (0.06 mol) and a spatula tip of tetrabutylammonium hydrogen sulfate, and the mixture is stirred for 18 hours at ambient temperature. The organic phase is separated, washed twice with water, and dried with sodium sulfate, and the methylene chloride is distilled off. The residue is purified by column chromatography [silica gel; chloroform/acetone (40:1)]. The uniform fractions are concentrated by evaporation, the residue is stirred with diisopropylether, and the crystal slurry is subjected to suction filtration and dried.

후처리

  1. customThe organic phase is separated
  2. washwashed twice with water
  3. dry with materialdried with sodium sulfate
  4. distillationthe methylene chloride is distilled off
  5. customThe residue is purified by column chromatography [silica gel; chloroform/acetone (40:1)]
  6. concentrationThe uniform fractions are concentrated by evaporation
  7. filtrationthe crystal slurry is subjected to suction filtration
  8. customdried

출처 및 근거

ORD 기록
ord-f2849dca1ed8412ab98283ff14962e73
출처 데이터셋
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04518597

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트