Hexane → HCID 131718352, 화합물

HRID 487333노트

반응식

HRID 487333 반응식
C([Li])CCC.CCCCCC.[C:12]([O:16][C:17]([NH:19][CH:20]1[CH2:29][CH2:28][C:27]2[C:22](=[CH:23][CH:24]=[C:25]([Br:30])[CH:26]=2)[CH2:21]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].[N:31]1[CH:36]=[CH:35][CH:34]=[C:33]([CH:37]=[O:38])[CH:32]=1>O1CCCC1>[C:12]([O:16][C:17]([NH:19][CH:20]1[CH2:29][CH2:28][C:27]2[CH2:26][C:25]([CH:37]([C:33]3[CH:32]=[N:31][CH:36]=[CH:35][CH:34]=3)[OH:38])([Br:30])[CH:24]=[CH:23][C:22]=2[CH2:21]1)=[O:18])([CH3:15])([CH3:13])[CH3:14]

참가 물질

6

반응물 4

HCID 8058HexaneHCID 103713-PyridinecarboxaldehydeHCID 10064926tert-butyl N-(6-bromo-1,2,3,4-tetrahydronaphthalen-2-yl)carbamateHCID 178418339Butyllithium

생성물 1

HCID 131718352HCID 131718352, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
-70 °C

실험 절차

8.8 ml of a solution of n-butyl lithium in hexane (2.5 mol) was dropped to a solution of 3.25 g of 2-tert.butoxycarbonylamino-6-bromo-1,2,3,4-tetrahydro-naphthaline in 50 ml of absolute tetrahydrofurane cooled to -70° C. and stirring was continued for 1.5 hours at -50° C. Subsequently, 1.1 g of pyridine-3-aldehyde were dropped into the mixture at -70° C. After stirring for one hour, the reaction mixture was poured on ice and extracted with ethyl acetate. The organic Phase was washed with water, dried and evaporated. The obtained residue was recrystallised from cyclohexane/ethyl acetate.

후처리

  1. stirringAfter stirring for one hour
  2. additionthe reaction mixture was poured on ice
  3. extractionextracted with ethyl acetate
  4. washThe organic Phase was washed with water
  5. customdried
  6. customevaporated
  7. customThe obtained residue was recrystallised from cyclohexane/ethyl acetate

출처 및 근거

ORD 기록
ord-7d105a01ba1a412a96298497fb66fbd6
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05294626

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