Methyl Bromide → 1,1′-[(1Z,3Z)-2,3-Diisocyano-1,3-butadiene-1,4-diyl]bis[4-methoxybenzene]

HRID 1033764노트

반응식

HRID 1033764 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[C:10](\[N+:22]#[C-:23])/[C:11](/[N+:20]#[C-:21])=[CH:12]/[C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=2)=[CH:5][CH:4]=1.[C:24](=O)([O-])[O-].[K+].[K+].CBr>CN(C=O)C>[CH3:24][O:19][C:16]1[CH:15]=[CH:14][C:13](/[CH:12]=[C:11](/[C:10](/[N+:22]#[C-:23])=[CH:9]/[C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=2)\[N+:20]#[C-:21])=[CH:18][CH:17]=1

참가 물질

5

반응물 3

HCID 6323Methyl BromideHCID 11430Potassium CarbonateHCID 6441021xanthocillin X monomethyl ether

생성물 1

HCID 64444531,1′-[(1Z,3Z)-2,3-Diisocyano-1,3-butadiene-1,4-diyl]bis[4-methoxybenzene]수율 110.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

13 mg of xanthocillin X monomethyl ether is dissolved in 2 ml of DMF and 40 mg of potassium carbonate is added thereto. Further, 50 μl of methyl bromide is added thereto and the mixture thus formed is extracted with 30 ml portions of ethyl acetate thrice. The extracts are combined, successively washed with water and a saturated aqueous solution of sodium chloride and dried over sodium sulfate. The sodium sulfate is filtered off, and the solvent is distilled from the filtrate. Thus, approximately 15 mg of xanthocillin X dimethylether is obtained in the form of a yellow solid.

후처리

  1. customthe mixture thus formed
  2. extractionis extracted with 30 ml portions of ethyl acetate thrice
  3. washsuccessively washed with water
  4. dry with materiala saturated aqueous solution of sodium chloride and dried over sodium sulfate
  5. filtrationThe sodium sulfate is filtered off
  6. distillationthe solvent is distilled from the filtrate

출처 및 근거

ORD 기록
ord-d829a9f6a9e3427fb3b337f5dbb314b0
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05312833

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