Hydrochloric Acid → Ethyl 2-(5-benzylthio-2-nitrophenoxy)acetate

HRID 1587354노트

반응식

HRID 1587354 반응식
F[C:2]1[CH:3]=[CH:4][C:5]([N+:15]([O-:17])=[O:16])=[C:6]([CH:14]=1)[O:7][CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10].[CH2:18]([SH:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(N(CC)CC)C.Cl>O.CN(C=O)C>[CH2:18]([S:25][C:2]1[CH:3]=[CH:4][C:5]([N+:15]([O-:17])=[O:16])=[C:6]([CH:14]=1)[O:7][CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 7509Benzyl mercaptanHCID 8471TriethylamineHCID 13752803Ethyl 2-(5-fluoro-2-nitrophenoxy)acetate

생성물 1

HCID 18994386Ethyl 2-(5-benzylthio-2-nitrophenoxy)acetate수율 72.9%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A mixture of ethyl 2-(5-fluoro-2-nitrophenoxy)acetate (11 g), benzylmercaptan (5.2 g), triethylamine (5.08 g) and DMF (50 ml) was stirred and heated to 80° C. for 7 hours. The mixture was cooled, poured into water and acidified by the addition of dilute aqueous hydrochloric acid. The mixture was extracted with diethyl ether. The organic phase was washed with water and with brine, dried (MgSO4) and evaporated to give ethyl 2-(5-benzylthio-2-nitrophenoxy)acetate (10.6 g, 68%) as a solid.

후처리

  1. temperatureThe mixture was cooled
  2. extractionThe mixture was extracted with diethyl ether
  3. washThe organic phase was washed with water and with brine
  4. dry with materialdried (MgSO4)
  5. customevaporated

출처 및 근거

ORD 기록
ord-d7e4bfd4c205404da930f62ed3aac7a7
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05217969

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