Hydrochloric Acid → Ethyl 9-(2,3-Dichlorophenyl)-1,1-dioxo-2,3,4,5,6,9-hexahydro-7-methylpyrido-[2,3-f][1,4]thiazepine-8-carboxylate

HRID 1461475ノート

反応式

HRID 1461475 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH:9]1[C:19]2[S:18](=[O:21])(=[O:20])[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14][C:13]=2[NH:12][C:11]([CH3:29])=[C:10]1[C:30]([O:32][CH2:33][CH3:34])=[O:31].Cl.[OH-].[Na+]>C(OCC)(=O)C>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH:9]1[C:19]2[S:18](=[O:20])(=[O:21])[CH2:17][CH2:16][NH:15][CH2:14][C:13]=2[NH:12][C:11]([CH3:29])=[C:10]1[C:30]([O:32][CH2:33][CH3:34])=[O:31]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 15035858HCID 15035858、化合物

生成物 1

HCID 15035859Ethyl 9-(2,3-Dichlorophenyl)-1,1-dioxo-2,3,4,5,6,9-hexahydro-7-methylpyrido-[2,3-f][1,4]thiazepine-8-carboxylate収率 94%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of ethyl 9-(2,3-dichlorophenyl)-4-(t-butyloxycarbonyl)-1,1-dioxo-2,3,4,5,6,9-hexahydro-7-methylpyrido[2,3-f][1,4]thiazepine-8-carboxylate (2.45 g, 4.6 mmole) from Example 7, in ethyl acetate (150 mL) was cooled to 0° C. and saturated with gaseous hydrogen chloride. The mixture was warmed to room temperature. The reaction was then again chilled to 0° C. and shaken with 200 mL of cold 4 N NaOH. The aqueous layer was separated and extracted with 2×100 mL of chloroform. The ethyl acetate layer was dried with brine and the combined organic extracts were dried over Na2SO4. The solvents were evaporated under reduced pressure and the residue triturated with ether to give the product (1.86 g, 94% yield).

後処理

  1. temperatureThe reaction was then again chilled to 0° C.
  2. customThe aqueous layer was separated
  3. extractionextracted with 2×100 mL of chloroform
  4. dry with materialThe ethyl acetate layer was dried with brine
  5. dry with materialthe combined organic extracts were dried over Na2SO4
  6. customThe solvents were evaporated under reduced pressure
  7. customthe residue triturated with ether

出典と根拠

ORDレコード
ord-fb2420e71e6149429b9917273ee2bf1a
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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