4,5,6,7-Tetrahydro-5-methyl-1,3-isobenzofurandione → HCID 22013583, 화합물

HRID 1532559노트

반응식

HRID 1532559 반응식
[Cl:1][CH:2]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:3][C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][C:10]=1[Cl:11])[NH2:7].[CH3:17][CH:18]1[CH2:28][CH2:27][C:21]2[C:22]([O:24][C:25](=O)[C:20]=2[CH2:19]1)=[O:23]>>[Cl:11][C:10]1[CH:9]=[CH:8][C:6]([N:7]2[C:25](=[O:24])[C:20]3[CH2:19][CH:18]([CH3:17])[CH2:28][CH2:27][C:21]=3[C:22]2=[O:23])=[CH:5][C:4]=1[CH2:3][CH:2]([Cl:1])[C:12]([O:14][CH2:15][CH3:16])=[O:13]

참가 물질

3

반응물 2

HCID 1181314,5,6,7-Tetrahydro-5-methyl-1,3-isobenzofurandioneHCID 22013609HCID 22013609, 화합물

생성물 1

HCID 22013583HCID 22013583, 화합물

실험 절차

2.60 g of 3-(2-chloro-2-ethoxycarbonyleth-1-yl)-4-chloroaniline and 1.65 g of 4-methyl-3,4,5,6-tetrahydrophthalic anhydride were refluxed for 6 hours. After the mixture had been cooled and evaporated down, the residue was taken up in ethyl acetate and the solution was washed three times with water. The organic phase was dried over Na2SO, and then evaporated down. Yield 3.0 g (75%); 1H-NMR (in d6-DMSO/TMS): δ [ppm]=0.96 (d; 3H), 1.05 (t; 3H), 1.64-2.08 (m; 3H), 2.15-2.70 (m; 4H), 3.20-3.55 (m; 2H), 4.14 (q; 2H), 4.78 (dd; 1H), 7.26 (d; 1H), 7.34 (s; 1H), 7.55 (d; 1H).

후처리

  1. temperatureAfter the mixture had been cooled
  2. customevaporated down
  3. washthe solution was washed three times with water
  4. dry with materialThe organic phase was dried over Na2SO
  5. customevaporated down

출처 및 근거

ORD 기록
ord-c904efaffff64b9785a9913fb18980a3
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06204222B1

반응 노트

불러오는 중…