Potassium Carbonate → HCID 11060875, 화합물

HRID 1531316

반응식

HRID 1531316 반응식
[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

참가 물질

12

반응물 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)acetate2회HCID 117916034-Cyclopentyloxy-3,5-dimethoxybenzaldehydeHCID 12986345Ethyl 2-(3,4-diaminophenyl)acetate

생성물 1

HCID 11060875HCID 11060875, 화합물

시약·촉매·용매 4

HCID 176Acetic Acid용매HCID 180Acetone용매HCID 702Ethanol용매HCID 1140Toluene용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-17a359feab954b548052de3d5d6c93ea
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06197800B1

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