Stannous chloride dihydrate → 5-Amino-2-iodobenzamide

HRID 503687

반응식

HRID 503687 반응식
O.O.[Sn](Cl)Cl.[I:6][C:7]1[CH:15]=[CH:14][C:13]([N+:16]([O-])=O)=[CH:12][C:8]=1[C:9]([NH2:11])=[O:10]>CN(C=O)C>[NH2:16][C:13]1[CH:14]=[CH:15][C:7]([I:6])=[C:8]([CH:12]=1)[C:9]([NH2:11])=[O:10]

참가 물질

4

반응물 2

HCID 61436Stannous chloride dihydrateHCID 98039472-Iodo-5-nitrobenzamide

생성물 1

HCID 155476225-Amino-2-iodobenzamide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

15.1 g (67 mmol) of tin(II) chloride dihydrate are added to a solution of 4.9 g (16.8 mmol) of the compound from Example 3A in 200 ml of DMF. The reaction mixture is stirred at 50° C. for one hour, and then the DMF is removed in vacuo. The residue is partitioned between 1 l of ethyl acetate and water, the phases are separated, and the organic phase is discarded. The aqueous phase is basified with 10% strength sodium hydroxide solution and again extracted with 500 ml of ethyl acetate. The product is dried over magnesium sulfate, filtered with suction and concentrated in vacuo. 3.95 g (90% of theory) of the title compound are obtained and are reacted without further purification in the next stage.

후처리

  1. customthe DMF is removed in vacuo
  2. customThe residue is partitioned between 1 l of ethyl acetate and water
  3. customthe phases are separated
  4. extractionagain extracted with 500 ml of ethyl acetate
  5. dry with materialThe product is dried over magnesium sulfate
  6. filtrationfiltered with suction
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-47fbc14711a846ac98ef725b6cda40b4
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776922B2

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