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Ethyl Acetate → 4-(1-(5-Hydroxymethylfur-2-ylmethyl)-1H-benzimidazol-2-yl)[1,4]diazepane

HRID 637072
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HRID 637072 반응식
C(OC([N:6]1[CH2:12][CH2:11][CH2:10][N:9]([C:13]2[N:17]([CH2:18][C:19]3[O:20][C:21]([CH2:24][OH:25])=[CH:22][CH:23]=3)[C:16]3[CH:26]=[CH:27][CH:28]=[CH:29][C:15]=3[N:14]=2)[CH2:8][CH2:7]1)=O)C.[OH-].[Na+].C(OCC)(=O)C>C(O)(C)C>[OH:25][CH2:24][C:21]1[O:20][C:19]([CH2:18][N:17]2[C:16]3[CH:26]=[CH:27][CH:28]=[CH:29][C:15]=3[N:14]=[C:13]2[N:9]2[CH2:10][CH2:11][CH2:12][NH:6][CH2:7][CH2:8]2)=[CH:23][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 184645131-ethoxycarbonyl-4-(1-(5-hydroxymethylfur-2-ylmethyl)-1H-benzimidazol-2-yl)[1,4]diazepane

생성물 1

HCID 184649364-(1-(5-Hydroxymethylfur-2-ylmethyl)-1H-benzimidazol-2-yl)[1,4]diazepane

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

Combine 1-ethoxycarbonyl-4-(1-(5-hydroxymethylfur-2-ylmethyl)-1H-benzimidazol-2-yl)[1,4]diazepane (4 mmol) and sodium hydroxide (8 mmol) in isopropanol (20 mL). Heat to reflux. After 2 days, evaporate the reaction mixture in vacuo to give a residue. Combine the residue and ethyl acetate. Extract with water and brine. Dry the organic layer over Na2SO4, filter, and evaporate in vacuo to give the title compound.

후처리

  1. temperatureHeat to reflux
  2. customevaporate the reaction mixture in vacuo
  3. customto give a residue
  4. extractionExtract with water and brine
  5. dry with materialDry the organic layer over Na2SO4
  6. filtrationfilter
  7. customevaporate in vacuo

출처 및 근거

ORD 기록
ord-dc0e8e76d9ad47c4ad21740dbecddae8
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06194406B1

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