Hydrochloric Acid → HCID 69300805, 화합물

HRID 131285노트

반응식

HRID 131285 반응식
[CH2:1]([NH:8][C:9]1[CH:19]=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:20][CH2:21][CH2:22][CH2:23][C:24](Cl)=[O:25].C(N(CC)C(C)C)(C)C.Cl>C(Cl)Cl.C(Cl)(Cl)Cl>[CH2:1]([N:8]([C:9]1[CH:10]=[CH:11][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:18][CH:19]=1)[C:24](=[O:25])[CH2:23][CH2:22][CH2:21][Cl:20])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 783704-Chlorobutyryl chlorideHCID 81531DiisopropylethylamineHCID 3832836Ethyl 4-(benzylamino)benzoate

생성물 1

HCID 69300805HCID 69300805, 화합물

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

To a solution of ethyl 4-benzylaminobenzoate (6.0 g) in methylene chloride (60 mL) is added dropwise chlorobutyryl chloride (3.95 mL) and N,N-diisopropylethylamine (6.14 mL) under ice-cooling, and the mixture is stirred for 12 hours. The reaction mixture is diluted with chloroform and thereto is added 10% HCl. The organic layer is separated, washed successively with water, a saturated sodium hydrogencarbonate solution, water, and saturated brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The residue is purified by flash column chromatography on silica gel (Solvent; n-hexane:ethyl acetate=4:1) to give ethyl 4-[N-benzyl-N-(4-chlorobutyryl)amino]benzoate (8.27 g, yield; quantitative) as an oil. MS (APCI) m/z; 360/362 [M+H]+

후처리

  1. temperaturecooling
  2. customThe organic layer is separated
  3. washwashed successively with water
  4. dry with materiala saturated sodium hydrogencarbonate solution, water, and saturated brine, dried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe residue is purified by flash column chromatography on silica gel (Solvent; n-hexane:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-3a129cab96f347c082e7fba86edc7c97
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07384952B2

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