中国医药工业杂志
中國醫藥工業雜誌
중국의약공업잡지
CHINESE JOURNAL OF PHARMACEUTICALS
2010年
2期
85-87
,共3页
李宗圣%Michael H.CHEN
李宗聖%Michael H.CHEN
리종골%Michael H.CHEN
(R)-3-氨基-2,3,4,5-四氢-1H[1]-2-氧代苯并氮杂(艹卓)%生长激素促分泌素%中间体%拆分%合成
(R)-3-氨基-2,3,4,5-四氫-1H[1]-2-氧代苯併氮雜(艸卓)%生長激素促分泌素%中間體%拆分%閤成
(R)-3-안기-2,3,4,5-사경-1H[1]-2-양대분병담잡(초탁)%생장격소촉분비소%중간체%탁분%합성
(R)-3-amino-2,3,4,5-tetrahydro-1H-[1]-2-oxobenzazepin%growth hormone secretagogue%intermediate%resolution%synthesis
3,4-二氢-2H-萘-1-酮与盐酸羟胺反应后,在PPA中经Beckmann重排、碘代得到3-碘代-2,3,4,5-四氢-1H-[1]-2-氧代苯并氮杂(5),5经氨解、D-焦谷氨酸拆分、浓氨水处理后催化氢化还原,得到(R)-3-氨基-2,3,4,5-四氢-1H[1]-2-氧代苯并氮杂(艹卓),总收率约44%,纯度98%,ee值99.5%.
3,4-二氫-2H-萘-1-酮與鹽痠羥胺反應後,在PPA中經Beckmann重排、碘代得到3-碘代-2,3,4,5-四氫-1H-[1]-2-氧代苯併氮雜(5),5經氨解、D-焦穀氨痠拆分、濃氨水處理後催化氫化還原,得到(R)-3-氨基-2,3,4,5-四氫-1H[1]-2-氧代苯併氮雜(艸卓),總收率約44%,純度98%,ee值99.5%.
3,4-이경-2H-내-1-동여염산간알반응후,재PPA중경Beckmann중배、전대득도3-전대-2,3,4,5-사경-1H-[1]-2-양대분병담잡(5),5경안해、D-초곡안산탁분、농안수처리후최화경화환원,득도(R)-3-안기-2,3,4,5-사경-1H[1]-2-양대분병담잡(초탁),총수솔약44%,순도98%,ee치99.5%.
(R)-3-Amino-2,3,4,5-tetrahydro-IH-[I]-2-oxobenzazepin was synthesized by reaction from 3,4-dihydro-2H-naphthalen-1-one by reaction with hydroxylamine hydrochloride.Beckmann rearrangement in PPA and iodination with HMDS/I_2 to give 3-iodo-2,3,4,5-tetrahydro-1H[1]-2-oxobenzazepin,which was subjected to ammonolysis,resolution with D-pyroglutamic acid,treatment with NH_3·H_2O and then catalytic hydrogenated reduction.The overall yield was about 44%.with 98%purity and 99.5%ee.
