Ethanol → HCID 21892028, 화합물

HRID 1250720노트

반응식

HRID 1250720 반응식
C([CH:3]([C:7]([Cl:9])=O)C(Cl)=O)C.[Cl:10][C:11]1[C:12]([O:22][CH3:23])=[CH:13][CH:14]=[C:15]([CH:21]=1)[NH:16][C:17](=[O:20])[CH2:18]Cl.C(N(CC)CC)C.[CH2:31]([O-:33])[CH3:32].[Na+].[CH2:35]([OH:37])C>C(#N)C.O>[Cl:10][C:11]1[CH:21]=[C:15]2[C:14]([C:3]([CH2:7][Cl:9])=[C:18]([C:35]([O:33][CH2:31][CH3:32])=[O:37])[C:17](=[O:20])[NH:16]2)=[CH:13][C:12]=1[O:22][CH3:23]

참가 물질

8

반응물 5

HCID 702EthanolHCID 8471TriethylamineHCID 24048042-chloro-N-(3-chloro-4-methoxyphenyl)acetamideHCID 2723922Sodium ethoxideHCID 109209242-Ethylpropanedioyl dichloride

생성물 1

HCID 21892028HCID 21892028, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

A solution of ethylmalonyl chloride (17 ml, 131 mmol) is added dropwise under argon and at 0° C. to a solution of 5-chloro-2-chloroacetyl-4-methoxyaniline (17 g, 73 mmol) and triethylamine (18.5 ml, 131 mmol) in anhydrous acetonitrile (310 ml). Agitation is carried out for 2 hours at ambient temperature, then a solution of sodium ethanolate in ethanol (obtained by 1.88 g, 80 mmol, of sodium in 90 ml of ethanol) is added dropwise at 0° C. Agitation is carried out for 12 hours at ambient temperature. 300 ml of water is added, and agitation is again carried out for 20 minutes. The precipitate is filtered out; washed with water, with ethanol, and with ethyl ether. After drying under vacuum 16.7 g of a yellowish solid is obtained.

후처리

  1. waitAgitation is carried out for 12 hours at ambient temperature
  2. waitagitation is again carried out for 20 minutes
  3. filtrationThe precipitate is filtered out
  4. washwashed with water, with ethanol
  5. dry with materialAfter drying under vacuum 16.7 g of a yellowish solid
  6. customis obtained

출처 및 근거

ORD 기록
ord-7be6534c8b5341dfaafc9d06fcb96636
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06339091B1

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