Hydrochloric Acid → (r)-6,8-Dibromochroman-4-amine hydrochloride

HRID 1008960ノート

反応式

HRID 1008960 の反応式
[N:1]([C@H:4]1[C:13]2[C:8](=[C:9]([Br:15])[CH:10]=[C:11]([Br:14])[CH:12]=2)[O:7][CH2:6][CH2:5]1)=[N+]=[N-].CP(C)C.[ClH:20]>O1CCCC1.C(#N)C>[ClH:20].[Br:14][C:11]1[CH:12]=[C:13]2[C:8](=[C:9]([Br:15])[CH:10]=1)[O:7][CH2:6][CH2:5][C@H:4]2[NH2:1]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 68983TrimethylphosphineHCID 866200164(R)-Azido-6,8-dibromo-chroman

生成物 1

HCID 67303951(r)-6,8-Dibromochroman-4-amine hydrochloride

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To an ice cooled solution of 4(R)-azido-6,8-dibromo-chroman in tetrahydrofuran (0.16M) was added 1.2 equivalents of trimethylphosphine. The mixture was warmed to room temperature and maintained for 16 h. Concentration of the mixture gave the crude amine. This was dissolved in acetonitrile (0.20M) and 2 equivalents of hydrochloric acid added. The mixture was stirred for 16 h and the solids filtered, washed with acetonitrile and dried to afford the title compound as an off-white solid.

後処理

  1. temperaturemaintained for 16 h
  2. customConcentration of the mixture gave the crude amine
  3. filtrationthe solids filtered
  4. washwashed with acetonitrile
  5. customdried

出典と根拠

ORDレコード
ord-54eb609add124280b639e552de9d8428
出典データセット
uspto-grants-2011_07
特許番号
US07973050B2

反応ノート

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