Potassium Carbonate → HCID 11060875、化合物

HRID 1531316

反応式

HRID 1531316 の反応式
[CH:1]1([O:6][C:7]2[C:14]([O:15][CH3:16])=[CH:13][C:10]([CH:11]=O)=[CH:9][C:8]=2[O:17][CH3:18])[CH2:5][CH2:4][CH2:3][CH2:2]1.[N:19]1[S:20][N:21]=[C:22]2[CH:27]=[C:26]([CH:28]([CH2:34][C:35]([C:37]3[CH:42]=[CH:41][C:40]([O:43][CH3:44])=[CH:39][CH:38]=3)=[O:36])[C:29]([O:31]CC)=[O:30])[CH:25]=[CH:24][C:23]=12.N1SN=C2C=C(CC(OCC)=O)C=CC=12.C(=O)([O-])[O-].[K+].[K+].NC1C=C(CC(OCC)=O)C=CC=1N.S(=NC1C=CC=CC=1)=O.[Na]>CC(C)=O.C1(C)C=CC=CC=1.C(O)C.C(O)(=O)C>[N:19]1[S:20][N:21]=[C:22]2[CH:27]=[C:26]([C:28]3[C:29](=[O:30])[O:31][C:35]([OH:36])([C:37]4[CH:38]=[CH:39][C:40]([O:43][CH3:44])=[CH:41][CH:42]=4)[C:34]=3[CH2:11][C:10]3[CH:13]=[C:14]([O:15][CH3:16])[C:7]([O:6][CH:1]4[CH2:5][CH2:4][CH2:3][CH2:2]4)=[C:8]([O:17][CH3:18])[CH:9]=3)[CH:25]=[CH:24][C:23]=12

参加物

12

反応物 7

HCID 11430Potassium CarbonateHCID 70739Benzenamine, N-sulfinyl-HCID 5360545SodiumHCID 10926758Ethyl 2-(2,1,3-benzothiadiazol-5-yl)-4-(4-methoxyphenyl)-4-oxobutanoateHCID 11127870ethyl 2-(2,1,3-benzothiadiazol-5-yl)acetate2 回HCID 117916034-Cyclopentyloxy-3,5-dimethoxybenzaldehydeHCID 12986345Ethyl 2-(3,4-diaminophenyl)acetate

生成物 1

HCID 11060875HCID 11060875、化合物

試薬・触媒・溶媒 4

HCID 176Acetic Acid溶媒HCID 180Acetone溶媒HCID 702Ethanol溶媒HCID 1140Toluene溶媒

実験手順

0.368 g of 4-cyclopentyloxy-3,5-dimethoxybenzaldehyde (“A”) and 0.52 g of ethyl 2-(2,1,3-benzothiadiazol-5-yl)-4-(4-methoxyphenyl)-4-oxobutanoate, m.p. 89° (obtainable by reaction of 5.5 g of ethyl 2-(2,1,3-benzothiadiazol-5-yl)acetate with 5.5 g of 2′-bromo-4-methoxyacetophenone and 4 g of potassium carbonate in 200 ml of acetone, 18 hours under reflux; ethyl 2-(2,1,3-benzothiadiazol-5-yl)acetate, m.p. 40-41° is obtained by reaction of 24.3 g of ethyl 3,4-diaminophenylacetate and 26.9 ml of thionylaniline in 80 ml of toluene, 4 hours under reflux) are added to a solution of 34 mg of sodium in 10 ml of ethanol and the mixture is heated under reflux for one hour. After addition of 1.4 ml of acetic acid, it is heated for a further 16 hours. The solvent is removed and the residue is worked up in the customary manner. 3-(2,1,3-Benzothiadiazol-5-yl)-4-(4-cyclopentyloxy-3,5-dimethoxy-benzyl)-5-hydroxy-5-(4-methoxyphenyl)-5H-furan-2-one is obtained, FAB 575.

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for one hour
  3. temperatureis heated for a further 16 hours
  4. customThe solvent is removed

出典と根拠

ORDレコード
ord-17a359feab954b548052de3d5d6c93ea
出典データセット
uspto-grants-2001_03
特許番号
US06197800B1

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