1-ethoxycarbonyl-4-(1-(5-(ethoxycarbonyl)fur-2-ylmethyl)-1H-benzimidazol-2-yl)[1,4]diazepane → 1-ethoxycarbonyl-4-(1-(5-hydroxymethylfur-2-ylmethyl)-1H-benzimidazol-2-yl)[1,4]diazepane

HRID 2230548노트

반응식

HRID 2230548 반응식
[CH2:1]([O:3][C:4]([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]([C:24](OCC)=[O:25])=[CH:22][CH:23]=3)[C:16]3[CH:29]=[CH:30][CH:31]=[CH:32][C:15]=3[N:14]=2)[CH2:8][CH2:7]1)=[O:5])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[CH2:1]([O:3][C:4]([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:29]=[CH:30][CH:31]=[CH:32][C:15]=3[N:14]=2)[CH2:8][CH2:7]1)=[O:5])[CH3:2]

참가 물질

4

반응물 2

HCID 184644291-ethoxycarbonyl-4-(1-(5-(ethoxycarbonyl)fur-2-ylmethyl)-1H-benzimidazol-2-yl)[1,4]diazepaneHCID 21226445Aluminium lithium hydride

생성물 1

HCID 184645131-ethoxycarbonyl-4-(1-(5-hydroxymethylfur-2-ylmethyl)-1H-benzimidazol-2-yl)[1,4]diazepane

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Combine 1-ethoxycarbonyl-4-(1-(5-(ethoxycarbonyl)fur-2-ylmethyl)-1H-benzimidazol-2-yl)[1,4]diazepane (5 mmol) and lithium aluminum hydride (5 mmol) in tetrahydrofuran. Heat to reflux. After 12 hour, cool and carefully quench the reaction mixture with 10% aqueous ammonium chloride solution. Extract the reaction mixture with ethyl acetate. Dry the the organic layer over Na2SO4, filter, and evaporate in vacuo to give 1-ethoxycarbonyl-4-(1-(5-hydroxymethylfur-2-ylmethyl)-1H-benzimidazol-2-yl)[1,4]diazepane.

후처리

  1. temperatureHeat to reflux
  2. temperaturecool
  3. customcarefully quench the reaction mixture with 10% aqueous ammonium chloride solution
  4. extractionExtract the reaction mixture with ethyl acetate
  5. dry with materialDry the the organic layer over Na2SO4
  6. filtrationfilter
  7. customevaporate in vacuo

출처 및 근거

ORD 기록
ord-8d933fb85f974a7399c05a0db2b27f92
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06423704B1

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