Chloride → HCID 14151761, 화합물

HRID 1088601노트

반응식

HRID 1088601 반응식
[S:1]1[C:5]([C:6](Cl)=[O:7])=[CH:4][C:3]2[CH:9]=[CH:10][CH:11]=[CH:12][C:2]1=2.S1C(C(O)=O)=CC2C=CC=CC1=2.C(Cl)(=O)C(Cl)=O.[NH2:31][CH:32]([P:41](=[O:48])([O:45][CH2:46][CH3:47])[O:42][CH2:43][CH3:44])[P:33](=[O:40])([O:37][CH2:38][CH3:39])[O:34][CH2:35][CH3:36].[Cl-]>C(Cl)Cl.CN(C)C1C=CN=CC=1.C(OCC)(=O)C.N1C=CC=CC=1>[S:1]1[C:5]([C:6]([NH:31][CH:32]([P:33](=[O:40])([O:34][CH2:35][CH3:36])[O:37][CH2:38][CH3:39])[P:41](=[O:48])([O:45][CH2:46][CH3:47])[O:42][CH2:43][CH3:44])=[O:7])=[CH:4][C:3]2[CH:9]=[CH:10][CH:11]=[CH:12][C:2]1=2

참가 물질

10

반응물 5

HCID 312ChlorideHCID 65578Oxalyl chlorideHCID 95864Benzo(b)thiophene-2-carboxylic acidHCID 142384Benzo[b]thiophene-2-carbonyl ChlorideHCID 2773808Tetraethyl aminomethylenediphosphonate

생성물 1

HCID 14151761HCID 14151761, 화합물

시약·촉매·용매 4

HCID 142844-(Dimethylamino)pyridine촉매HCID 1049Pyridine용매HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2-benzo[b]thiophenecarbonyl chloride prepared from 2-benzo[b]thiophenecarboxylic acid (356 mg) and oxalyl chloride (0.35 ml) in methylene chloride (2 ml) was added dropwise a mixture of tetraethyl (aminomethylene)bis(phosphonate) (606 mg), pyridine (316 mg) and trace amounts of 4-(dimethylamino)pyridine in methylene at 5° C. The mixture was stirred for 2 chloride (8 ml) hours at ambient temperature followed by the addition of ethyl acetate. The mixture was washed with water, 1N hydrochloric acid, saturated aqueous solution of sodium bicarbonate and brine successively. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The residue was treated with diisopropyl ether to give tetraethyl [(2-benzo[b]thiophenecarboxamido)-methylene]bis(phosphonate) (790 mg) as a white powder which was recrystallized from a mixture of ethyl acetate and n-hexane.

후처리

  1. additionwas added dropwise
  2. customat 5° C
  3. washThe mixture was washed with water, 1N hydrochloric acid, saturated aqueous solution of sodium bicarbonate and brine successively
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. additionThe residue was treated with diisopropyl ether

출처 및 근거

ORD 기록
ord-7f2b4c3127df459da2fe537ce27de6b0
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04963536

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