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

HRID 1008960노트

반응식

HRID 1008960 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-54eb609add124280b639e552de9d8428
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07973050B2

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