Diethylamine → HCID 86700071, compound

HRID 1428118Notes

Reaction equation

HRID 1428118 reaction equation
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].F[P-](F)(F)(F)(F)F.N1(O[P+](N2CCCC2)(N2CCCC2)N2CCCC2)C2C=CC=CC=2N=N1.[CH2:39]([O:41][C:42]([C:44]1[C:45](=[O:61])[C:46]([C:58](O)=[O:59])=[CH:47][N:48]([CH2:50][C:51]2[CH:56]=[CH:55][C:54]([F:57])=[CH:53][CH:52]=2)[CH:49]=1)=[O:43])[CH3:40]>ClCCl>[CH2:1]([N:3]([CH2:4][CH3:5])[C:58]([C:46]1[C:45](=[O:61])[C:44]([C:42]([O:41][CH2:39][CH3:40])=[O:43])=[CH:49][N:48]([CH2:50][C:51]2[CH:56]=[CH:55][C:54]([F:57])=[CH:53][CH:52]=2)[CH:47]=1)=[O:59])[CH3:2]

Participants

5

Reactant 3

HCID 8021DiethylamineHCID 2724699PyBOPHCID 86700072HCID 86700072, compound

Product 1

HCID 86700071HCID 86700071, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Diethylamine (130 μl) and 1H-benzotriazol-1-yloxytripyrrolidinophosphonium hexafluorophosphate (528 mg) were added to a solution of the compound obtained in Step 2 (270 mg) in dichloromethane (3.0 ml) at room temperature, and the mixture was stirred for five hours. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography [chloroform:methanol=300:1->30:1 (v/v)] to give 160 mg of the title compound as an oily substance.

Workup

  1. distillationThe solvent was distilled off under reduced pressure
  2. customthe residue was purified by silica gel column chromatography [chloroform:methanol=300:1->30:1 (v/v)]

Sources & evidence

ORD record
ord-9b4b74243b31461b84ed66c4f783fb33
Source dataset
uspto-grants-2015_01
Patent number
US08933103B2

Reaction notes

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