Triethylamine → HCID 72238040, 화합물

HRID 2370301노트

반응식

HRID 2370301 반응식
[CH2:1]1[O:14][C:4]2([CH2:11][CH2:10][CH:9]3[CH2:12][CH:5]2[CH2:6][CH2:7][CH:8]3[NH2:13])[O:3][CH2:2]1.C(N(CC)CC)C.[CH2:22]([O:29][C:30](Cl)=[O:31])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>ClCCl.O>[CH2:2]1[O:3][C:4]2([CH2:11][CH2:10][CH:9]3[CH2:12][CH:5]2[CH2:6][CH2:7][CH:8]3[NH:13][C:30]([O:29][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[O:31])[O:14][CH2:1]1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 72238032HCID 72238032, 화합물

생성물 1

HCID 72238040HCID 72238040, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

1.97 g of 6-Amino-bicyclo[3.3.1]nonan-2-one ethylene ketal (98) were dissolved in 30 mL of dry dichloromethane and 1.52 mL of dry triethylamine and 1.42 mL of benzylchloroformate were added. The mixture was stirred overnight, taken up in water and extracted three times with ethyl acetate. The combined organic layer was dried over sodium sulfate and evaporated to dryness. The crude product was purified by chromatography to give 0.92 g of the desired product. Rt=3.18 min (Method E). Detected mass: 332.2 (M+H+).

후처리

  1. extractionextracted three times with ethyl acetate
  2. dry with materialThe combined organic layer was dried over sodium sulfate
  3. customevaporated to dryness
  4. customThe crude product was purified by chromatography

출처 및 근거

ORD 기록
ord-5fd275a78d39462c993779ec4ef88bcc
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08710077B2

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