Isopropanol → HCID 19603840、化合物

HRID 2292490ノート

反応式

HRID 2292490 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([N+:19]([O-:21])=[O:20])=[C:13]([CH2:15][C:16]([OH:18])=[O:17])[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:22][CH:23](O)[CH3:24].Cl.C(N=C=NCCCN(C)C)C>C(Cl)Cl.CN(C)C1C=CN=CC=1>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([N+:19]([O-:21])=[O:20])=[C:13]([CH2:15][C:16]([O:18][CH:23]([CH3:24])[CH3:22])=[O:17])[CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 3776IsopropanolHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 19603791HCID 19603791、化合物

生成物 1

HCID 19603840HCID 19603840、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5-benzyloxy-2-nitrophenylacetic acid (25.1 g) in methylene chloride (250 ml) were added in turn 2-propanol (27 ml), 4-dimethylaminopyridine (1.07 and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (18.4 g) and the resulting mixture was stirred at room temperature for one hour and then allowed to stand overnight. After the solvent was distilled off under reduced pressure, the resulting residue was diluted with ethyl acetate, washed subsequently with 1N hydrochloric acid and saturated saline. The organic layer was dried over magnesium sulfate and distilled off under reduced pressure. The dark yellow oily substance thus obtained (29.7 g) was purified by a silica gel column chromatography (hexane:ethyl acetate=4:1) to give the title compound (22.5 g).

後処理

  1. waitto stand overnight
  2. distillationAfter the solvent was distilled off under reduced pressure
  3. additionthe resulting residue was diluted with ethyl acetate
  4. washwashed subsequently with 1N hydrochloric acid and saturated saline
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. distillationdistilled off under reduced pressure
  7. customThe dark yellow oily substance thus obtained (29.7 g)
  8. customwas purified by a silica gel column chromatography (hexane:ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-2e53e0f9c9804bdea1c91b5f03f68570
出典データセット
uspto-grants-1997_11
特許番号
US05684003

反応ノート

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