2,3-Dichlorobenzaldehyde → HCID 19980840、化合物

HRID 1461480ノート

反応式

HRID 1461480 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 19980840HCID 19980840、化合物収率 34.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-466761ee21084fa98a049d377c505574
出典データセット
uspto-grants-1991_12
特許番号
US05075440

反応ノート

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