2,3-Dichlorobenzaldehyde → HCID 19980840, 화합물

HRID 1461480노트

반응식

HRID 1461480 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:14][C:13](=[O:15])[CH2:12][S:11](=[O:17])(=[O:16])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl:18][C:19]1[C:26]([Cl:27])=[CH:25][CH:24]=[CH:23][C:20]=1[CH:21]=O.[NH2:28]/[C:29](/[CH3:37])=[CH:30]\[C:31]([O:33][CH2:34][CH2:35][OH:36])=[O:32]>C(O)C>[C:1]([O:5][C:6]([N:8]1[CH2:14][C:13]2([OH:15])[NH:28][C:29]([CH3:37])=[C:30]([C:31]([O:33][CH2:34][CH2:35][OH:36])=[O:32])[CH:21]([C:20]3[CH:23]=[CH:24][CH:25]=[C:26]([Cl:27])[C:19]=3[Cl:18])[CH:12]2[S:11](=[O:16])(=[O:17])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 357452,3-DichlorobenzaldehydeHCID 19980844tert-Butyl 6-oxo-1,4-thiazepane-4-carboxylate 1,1-dioxideHCID 19980851HCID 19980851, 화합물

생성물 1

HCID 19980840HCID 19980840, 화합물수율 34.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 4-N-(t-butyloxycarbonyl)-1,1-dioxo -2,3,4,5,6,7-hexahydro-1,4-thiazepine-6-one (9.06 g, 34.5 mmole) from Example 6, 2,3-dichlorobenzaldehyde (6.03 g, 34.5 mmole) and 2-hydroxyethyl 3-aminocrotonate (5.00 g, 34.5 mmole) was heated to reflux in 200 mL of ethanol for 24 hours. The ethanol was removed under reduced pressure and the residue was heated in refluxing toluene for 2 hours. After cooling a precipitate was filtered to give 6.75 g of the title compound. Evaporation of the filtrate and chromatography (2.5:1, ethyl acetate:hexane) produced 3.78 g of product.

후처리

  1. temperaturewas heated
  2. customThe ethanol was removed under reduced pressure
  3. temperaturethe residue was heated
  4. temperaturein refluxing toluene for 2 hours
  5. temperatureAfter cooling a precipitate
  6. filtrationwas filtered

출처 및 근거

ORD 기록
ord-466761ee21084fa98a049d377c505574
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05075440

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