Acetic Acid → HCID 178475827, compound

HRID 2068521Notes

Reaction equation

[F:1][C:2]([F:45])([F:44])[C:3]1[CH:4]=[C:5]([CH2:13][N:14]([C:38]2[N:39]=[N:40][N:41]([CH3:43])[N:42]=2)[C@@H:15]2[C:21]3[CH:22]=[C:23]([CH3:27])[CH:24]=[C:25]([CH3:26])[C:20]=3[N:19]([CH2:28][C@H:29]3[CH2:34][CH2:33][C@H:32]([C:35]([OH:37])=[O:36])[CH2:31][CH2:30]3)[CH2:18][CH2:17][CH2:16]2)[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.C(O)(=O)C>CCCCCCC>[C:35]([OH:37])(=[O:36])[CH3:32].[F:12][C:9]([F:10])([F:11])[C:7]1[CH:6]=[C:5]([CH2:13][N:14]([C:38]2[N:39]=[N:40][N:41]([CH3:43])[N:42]=2)[C@@H:15]2[C:21]3[CH:22]=[C:23]([CH3:27])[CH:24]=[C:25]([CH3:26])[C:20]=3[N:19]([CH2:28][C@H:29]3[CH2:34][CH2:33][C@H:32]([C:35]([OH:37])=[O:36])[CH2:31][CH2:30]3)[CH2:18][CH2:17][CH2:16]2)[CH:4]=[C:3]([C:2]([F:1])([F:45])[F:44])[CH:8]=1

Participants

Conditions

Temperature: 50 °C

Procedure

Suspend Trans-4-[[(5S)-5-[[[3,5-bis(trifluoromethyl)phenyl]methyl](2-methyl-2H-tetrazol-5-yl)amino]-2,3,4,5-tetrahydro-7,9-dimethyl-1H-1-benzazepin-1-yl]methyl]-cyclohexanecarboxylic acid (1.5 grams) in 10 mL of heptane. Heat the suspension to 50° C. Add 1 mL of acetic acid, and the suspension becomes clear. Add 10 ml more of heptane and cool to room temperature. Isolate the solid product by vacuum filtration and air-dry. The XRD spectrum was collected as described in Example 7. Table 3 below lists the peaks obtained from the XRD spectrum.

Workup

temperaturecool to room temperature
customIsolate the solid product
filtrationby vacuum filtration
customair-dry
customThe XRD spectrum was collected
customTable 3 below lists the peaks obtained from the XRD spectrum

Sources & evidence

ORD record: ord-a7ed1d8cde8e4a9d83dd3d51dd3e92d2
Source dataset: uspto-grants-2012_10
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08299060B2

Reaction notes

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