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Sodium Sulfate → HCID 22381739, 화합물

HRID 895776
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HRID 895776 반응식
[CH2:1]1[N:12]2[C:13]3[C:9]([C:10]4[CH2:16][CH2:15][CH2:14][C:11]=42)=[CH:8][CH:7]=[CH:6][C:5]=3[CH2:4][NH:3][C:2]1=O.[O-]S([O-])(=O)=O.[Na+].[Na+]>CCOCC.[H-].[H-].[H-].[H-].[Li+].[Al+3]>[CH:1]1[N:12]2[C:13]3[C:9]([C:10]4[CH2:16][CH2:15][CH2:14][C:11]=42)=[CH:8][CH:7]=[CH:6][C:5]=3[CH2:4][NH:3][CH:2]=1
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참가 물질

5

반응물 2

HCID 24436Sodium SulfateHCID 22381731HCID 22381731, 화합물

생성물 1

HCID 22381739HCID 22381739, 화합물수율 70%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매3회HCID 21226445Aluminium lithium hydride용매

실험 절차

To a suspension of 3,4,9,10-tetrahydro-8H-cyclopenta[b][1,4]diazepino[6,7,1-hi]indol-2(1H)-one (67 mg, 0.30 mmol) in Et2O (7 mL), LAH power (28 mg, 0.74 mmol) was added slowly at rt under Ar. After 16 h, additional Et2O (5 mL) was added followed by dropwise addition of a sat'd Na2SO4 solution (0.1 mL). H2 gas evolved upon addition. Additional Et2O (8 mL) was added, dried over Na2SO4, filtered and concentrated in vacuo to give 44 mg (70%) of the title compound as a yellow syrup.

후처리

  1. additionwas added slowly at rt under Ar
  2. additionH2 gas evolved upon addition
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e9935e178cea48f0965b18e469cc2e5d
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06916922B2

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