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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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tert-butyl (E)-[5-(3,4-dichlorostyryl)-2,3-dihydro-1-methyl-1H-1,4-benzodiazepin-7-yl]carbamate → (E)-5-(3,4-dichlorostyryl)-2,3-dihydro-1-methyl-1H-1,4-benzodiazepin-7-amine hydrochloride

HRID 48359
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인쇄 미리보기

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HRID 48359 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][C:29]=1[Cl:30])[CH:5]=[CH:6][C:7]1=[N:8][CH2:9][CH2:10][N:11]([CH3:26])[C:12]2[CH:17]=[CH:16][C:15]([NH:18]C(=O)OC(C)(C)C)=[CH:14][C:13]1=2>C(#N)C.C1(OC)C=CC=CC=1.FC(F)(F)C(O)=O>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][C:29]=1[Cl:30])[CH:5]=[CH:6][C:7]1=[N:8][CH2:9][CH2:10][N:11]([CH3:26])[C:12]2[CH:17]=[CH:16][C:15]([NH2:18])=[CH:14][C:13]1=2
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참가 물질

5

반응물 1

HCID 86585822tert-butyl (E)-[5-(3,4-dichlorostyryl)-2,3-dihydro-1-methyl-1H-1,4-benzodiazepin-7-yl]carbamate

생성물 1

HCID 69892163(E)-5-(3,4-dichlorostyryl)-2,3-dihydro-1-methyl-1H-1,4-benzodiazepin-7-amine hydrochloride수율 165.1%

시약·촉매·용매 3

HCID 6422Trifluoroacetic acid촉매HCID 7519Anisole촉매HCID 6342Acetonitrile
용매

실험 절차

To a solution of 11 mg (0.025 mmol) of tert-butyl (E)-[5-(3,4-dichlorostyryl)-2,3-dihydro-1-methyl-1H-1,4-benzodiazepin-7-yl]carbamate in 0.5 ml of acetonitrile and 1 drop of anisole was added 1 drop of trifluoroacetic acid. The solution was stirred for 20 minutes, concentrated under reduced pressure and the residue partitioned between brine and dichloromethane. The organic phase was dried over magnesium sulphate, filtered and evaporated, redissolved in a solution of hydrogen chloride in ethyl acetate and the solvent removed to afford 7.9 mg of (E)-5-(3,4-dichlorostyryl)-2,3-dihydro-1-methyl-1H-1,4-benzodiazepin-7-amine hydrochloride as a red solid MS: m/e 346.2 [M+H]+.

후처리

  1. concentrationconcentrated under reduced pressure
  2. customthe residue partitioned between brine and dichloromethane
  3. dry with materialThe organic phase was dried over magnesium sulphate
  4. filtrationfiltered
  5. customevaporated
  6. dissolutionredissolved in a solution of hydrogen chloride in ethyl acetate
  7. customthe solvent removed

출처 및 근거

ORD 기록
ord-1a2b4a40082f4f8983fca7ce2853d8bc
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06703387B2

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