Dichloromethane → HCID 72420802, compound

HRID 1371529Notes

Reaction equation

HRID 1371529 reaction equation
C(OC([N:8]1[CH:17]([C:18](=[O:52])[NH:19][CH:20]([C:45]2[CH:50]=[CH:49][C:48](Cl)=CC=2)[C:21]([N:23]2[CH2:28][CH2:27][CH:26]([C:29]3[C:38]4[CH2:37][CH:36]([N:39]5[CH2:44][CH2:43][O:42][CH2:41][CH2:40]5)[CH2:35][CH2:34][C:33]=4[CH:32]=[CH:31][CH:30]=3)[CH2:25][CH2:24]2)=[O:22])[CH2:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH2:9]1)=O)(C)(C)C.[C:53](O)([C:55](F)(F)F)=O.[CH2:60]([Cl:62])Cl>>[Cl:62][C:60]1[CH:48]=[CH:49][C:50]([CH2:45][CH:20]([NH:19][C:18]([CH:17]2[CH2:16][C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH2:9][NH:8]2)=[O:52])[C:21]([N:23]2[CH2:24][CH2:25][CH:26]([C:29]3[C:38]4[CH2:37][CH:36]([N:39]5[CH2:44][CH2:43][O:42][CH2:41][CH2:40]5)[CH2:35][CH2:34][C:33]=4[CH:32]=[CH:31][CH:30]=3)[CH2:27][CH2:28]2)=[O:22])=[CH:55][CH:53]=1

Participants

4

Reactant 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 69415525HCID 69415525, compound

Product 1

HCID 72420802HCID 72420802, compoundYield 94%

Procedure

To compound prepared in Example 19 (0.42 g, 0.567 mmol), in DCM (3 mL), is added TFA (3 mL) and the mixture is stirred at room temperature for about 45 minutes. After concentrating to dryness, the resulting residue is triturated with Et2O, and the resulting solid is collected by filtration and dried to afford about 0.47 g of the final product (94%). EIS-MS 641.2 [M+1]

Workup

  1. concentrationAfter concentrating to dryness
  2. customthe resulting residue is triturated with Et2O
  3. filtrationthe resulting solid is collected by filtration
  4. customdried

Sources & evidence

ORD record
ord-ddea48ceee2e49eb958b53cf01b860bb
Source dataset
uspto-grants-2007_01
Patent number
US07157463B2

Reaction notes

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