4,5,6,7-Tetrahydro-5-methyl-1,3-isobenzofurandione → HCID 22013583、化合物

HRID 398806ノート

反応式

HRID 398806 の反応式
[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]

参加物

3

反応物 2

HCID 1181314,5,6,7-Tetrahydro-5-methyl-1,3-isobenzofurandioneHCID 22013609HCID 22013609、化合物

生成物 1

HCID 22013583HCID 22013583、化合物

実験手順

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 Na2SO4 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).

後処理

  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 Na2SO4
  5. customevaporated down

出典と根拠

ORDレコード
ord-9ba5b09b1c564d40b721607a1f089433
出典データセット
uspto-grants-1998_10
特許番号
US05817603

反応ノート

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