Ammonium Chloride → HCID 67608818, compound

HRID 2063586Notes

Reaction equation

HRID 2063586 reaction equation
FC(F)(F)C(O)=O.[CH3:8][N:9]1[CH2:14][CH2:13][N:12]([C:15]2[CH:20]=[CH:19][C:18]([NH:21][C:22]3[N:23]=[CH:24][C:25]4[C:48](=[O:49])[N:29]5[N:30]([C:42]6[CH:47]=[CH:46][CH:45]=[CH:44][N:43]=6)[C:31]6[CH:32]=[C:33]([O:37][CH2:38][C:39](O)=[O:40])[CH:34]=[CH:35][C:36]=6[C:28]5=[N:27][C:26]=4[N:50]=3)=[CH:17][CH:16]=2)[CH2:11][CH2:10]1.[Cl-].[NH4+].Cl.C[N:55](C)CCCN=C=NCC.O.ON1C2C=CC=CC=2N=N1>C(N(CC)CC)C.CN(C)C=O>[CH3:8][N:9]1[CH2:10][CH2:11][N:12]([C:15]2[CH:20]=[CH:19][C:18]([NH:21][C:22]3[N:23]=[CH:24][C:25]4[C:48](=[O:49])[N:29]5[N:30]([C:42]6[CH:47]=[CH:46][CH:45]=[CH:44][N:43]=6)[C:31]6[CH:32]=[C:33]([O:37][CH2:38][C:39]([NH2:55])=[O:40])[CH:34]=[CH:35][C:36]=6[C:28]5=[N:27][C:26]=4[N:50]=3)=[CH:17][CH:16]=2)[CH2:13][CH2:14]1

Participants

7

Reactant 4

HCID 25517Ammonium ChlorideHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 66623987HCID 66623987, compound

Product 1

HCID 67608818HCID 67608818, compoundYield 50.4%

Reagents, catalysts & solvents 2

HCID 6228DimethylformamideSolventHCID 8471TriethylamineSolvent

Procedure

An N,N-dimethylformamide (1 mL) solution of the compound (10 mg) obtained in Example 157, ammonium chloride (5 mg), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (10 mg), 1-hydroxybenzotriazole monohydrate (7 mg) and triethylamine (0.05 mL) was stirred for 16 hours. The reaction liquid was concentrated under reduced pressure, and the precipitated solid was collected through filtration, washed with distilled water and ethyl acetate in that order, and dried to give the title compound as a yellow solid (4.2 mg).

Workup

  1. customThe reaction liquid
  2. concentrationwas concentrated under reduced pressure
  3. filtrationthe precipitated solid was collected through filtration
  4. washwashed with distilled water and ethyl acetate in that order
  5. customdried

Sources & evidence

ORD record
ord-88cf591718fd4b02b87ffb3faad8b896
Source dataset
uspto-grants-2012_10
Patent number
US08288396B2

Reaction notes

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