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 1461475노트

반응식

HRID 1461475 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 15035858HCID 15035858, 화합물

생성물 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-carboxylate수율 94%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-fb2420e71e6149429b9917273ee2bf1a
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05075440

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