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

HRID 1492151ノート

反応式

HRID 1492151 の反応式
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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-08f91ed493d54cc19c1d1860935260a7
出典データセット
uspto-grants-1994_12
特許番号
US05373007

反応ノート

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