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Hydrochloric Acid → (1,4-Diazepan-1-yl)(furan-2-yl)methanone

HRID 1703374
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반응식

HRID 1703374 반응식
[NH:1]1[CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl.[O:9]1[CH:13]=[CH:12][CH:11]=[C:10]1[C:14](Cl)=[O:15].[OH-].[Na+]>O>[O:9]1[CH:13]=[CH:12][CH:11]=[C:10]1[C:14]([N:1]1[CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1)=[O:15]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2회HCID 68163Hexahydro-1,4-diazepineHCID 682422-Furancarbonyl chloride

생성물 1

HCID 12694336(1,4-Diazepan-1-yl)(furan-2-yl)methanone

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Homopiperazine (70 g., 0.70 mole) in 160 ml. water was treated with 6 N hydrochloric acid to adjust to pH 5.5 Furoyl chloride (79.5 g., 0.60 mole) and 25% (w/w) aqueous sodium hydroxide solution were added simultaneously to maintain a pH of 4.5-5.5. Then additional sodium hydroxide was added to bring the mixture to pH 9.5. The solution was extracted with chloroform, dried over anhydrous potassium carbonate and distilled to afford 63 g. of product, B.P. 124°-130° C. at 10 mm.

후처리

  1. additionwere added simultaneously
  2. temperatureto maintain a pH of 4.5-5.5
  3. extractionThe solution was extracted with chloroform
  4. dry with materialdried over anhydrous potassium carbonate
  5. distillationdistilled
  6. customto afford 63 g

출처 및 근거

ORD 기록
ord-497c6fabe0124a15969c17ee38de26a5
출처 데이터셋
uspto-grants-1982_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04351940

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