8-Benzyl-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine → 6,7,8,9-Tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine

HRID 518110Notes

Reaction equation

C([N:8]1[CH2:14][C:13]2[N:15]=[CH:16][C:17]([NH2:19])=[N:18][C:12]=2[O:11][CH2:10][CH2:9]1)C1C=CC=CC=1>[OH-].[OH-].[Pd+2].CO>[N:15]1[C:13]2[CH2:14][NH:8][CH2:9][CH2:10][O:11][C:12]=2[N:18]=[C:17]([NH2:19])[CH:16]=1

Participants

Conditions

Temperature: 50 °C

Procedure

A mixture of 8-benzyl-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine (87 mg), 20% Pd(OH)2/C (150 mg) and methanol (2 ml) was stirred under a hydrogen atmosphere at 50° C. for 1 hr. Insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by recrystallization (ethanol-hexane) to give the title compound (19.7 mg, 35%) as colorless crystals.

Workup

filtrationInsoluble material was filtered off
concentrationthe filtrate was concentrated under reduced pressure
customThe residue was purified by recrystallization (ethanol-hexane)

Sources & evidence

ORD record: ord-7818f9a4bd9e472b83691ead503744eb
Source dataset: uspto-grants-2015_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09115139B2

Reaction notes

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