Hydrochloric Acid → HCID 67422368, 화합물

HRID 880706노트

반응식

HRID 880706 반응식
C([Li])CCC.[C:6]([N:13]1[CH2:16][C:15](=[O:17])[CH2:14]1)([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7].Cl.[CH2:19]([O:26][C:27]1[CH:32]=[C:31]([O:33][CH2:34][C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH:30]=[CH:29][C:28]=1Br)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>O1CCCC1.CCCCCC>[C:9]([O:8][C:6]([N:13]1[CH2:16][C:15]([C:30]2[CH:29]=[CH:28][C:27]([O:26][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[CH:32][C:31]=2[O:33][CH2:34][C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=2)([OH:17])[CH2:14]1)=[O:7])([CH3:12])([CH3:11])[CH3:10]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 15194043-Oxo-azetidine-1-carboxylic acid tert-butyl esterHCID 128821681,1'-[(4-Bromo-1,3-phenylene)bis(oxymethylene)]dibenzeneHCID 178418339Butyllithium

생성물 1

HCID 67422368HCID 67422368, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8058Hexane용매

반응 조건

온도
-70 °C

실험 절차

In a 100 ml three-necked flask, 5 g of 2,4-bis(benzyloxy)-1-bromobenzene are dissolved in 60 ml of tetrahydrofuran. The mixture is cooled to −70° C. and then 11.4 ml of 2.5M n-butyllithium in hexane are added. The reaction medium is stirred at −70° C. for 1 hour, and then 2.8 g of 1-Boc-azetidine-3-one dissolved in 4 ml of THF are added dropwise. The reaction medium is stirred at −70° C. for 2 hours and then left at ambient temperature overnight. The reaction medium is poured into 40 ml of a 2M solution of hydrochloric acid and then extracted with 100 ml of ethyl acetate. The organic phases are combined, washed with 50 ml of water and then dried over magnesium sulphate and evaporated.

후처리

  1. additionare added dropwise
  2. stirringThe reaction medium is stirred at −70° C. for 2 hours
  3. waitleft at ambient temperature overnight
  4. extractionextracted with 100 ml of ethyl acetate
  5. washwashed with 50 ml of water
  6. dry with materialdried over magnesium sulphate
  7. customevaporated

출처 및 근거

ORD 기록
ord-a463b4c52e574cdda0e2416a0eab7c57
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993596B2

반응 노트

불러오는 중…