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Tributyltin azide → HCID 178519601, compound

HRID 2417544
Notes
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Reaction equation

HRID 2417544 reaction equation
[Cl:1][C:2]1[CH:37]=[CH:36][C:5]([C:6]([N:8]2[CH2:14][C:13]3[CH:15]=[C:16]([C:19]#[N:20])[CH:17]=[CH:18][C:12]=3[N:11]([CH2:21][C:22]3[CH:27]=[CH:26][C:25]([C:28]([N:30]4[CH2:34][CH:33]=[CH:32][CH2:31]4)=[O:29])=[CH:24][CH:23]=3)[C:10](=[O:35])[CH2:9]2)=[O:7])=[CH:4][CH:3]=1.C([Sn]([N:51]=[N+:52]=[N-:53])(CCCC)CCCC)CCC>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([N:8]2[CH2:14][C:13]3[CH:15]=[C:16]([C:19]4[NH:53][N:52]=[N:51][N:20]=4)[CH:17]=[CH:18][C:12]=3[N:11]([CH2:21][C:22]3[CH:27]=[CH:26][C:25]([C:28]([N:30]4[CH2:31][CH:32]=[CH:33][CH2:34]4)=[O:29])=[CH:24][CH:23]=3)[C:10](=[O:35])[CH2:9]2)=[O:7])=[CH:36][CH:37]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 4984872Tributyltin azideHCID 22632586HCID 22632586, compound

Product 1

HCID 178519601HCID 178519601, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
100 °C

Procedure

26 mg (0.051 mmol) of 4-(4-chlorobenzoyl)-7-cyano-1-[4-(2,5-dihydro-1H-pyrrol-1-ylcarbonyl)benzyl]-1,3,4,5-tetrahydrobenzo[e][1,4]-diazepin-2-on was dissolved in 10 ml of toluene. 0.032 ml (0.11 mmol) of tributyltin azide was added to the obtained solution, and they were stirred at 100° C. overnight. After the treatment with ethyl acetate as the extracting solvent by an ordinary method, the solvent was evaporated and the obtained crude product was treated in the same manner as in Step 3 in Example 1 to obtain the title compound.

Workup

  1. customAfter the treatment with ethyl acetate as the extracting solvent by an ordinary method, the solvent was evaporated
  2. customthe obtained crude product
  3. additionwas treated in the same manner as in Step 3 in Example 1

Sources & evidence

ORD record
ord-15c2a0353d2d4b688bd2348224dbb302
Source dataset
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06825191B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes