Calcium Carbonate → HCID 22916682, 화합물

HRID 1376616

반응식

HRID 1376616 반응식
[C:1]([O:5][C:6]([NH:8][CH2:9][C:10](=[S:12])[NH2:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl[CH:14]([C:20]([CH3:22])=O)[C:15]([O:17][CH2:18][CH3:19])=[O:16].C(=O)([O-])[O-].[Ca+2]>C(O)C>[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]1[S:12][C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[C:20]([CH3:22])[N:11]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 10112Calcium CarbonateHCID 11858Ethyl 2-chloroacetoacetateHCID 5324304tert-butyl N-(carbamothioylmethyl)carbamate

생성물 1

HCID 22916682HCID 22916682, 화합물수율 71%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
50 °C

실험 절차

To a solution of 5.02 g of (tert-butoxycarbonylamino)acetothioamide in 75 ml of ethanol were added 3.92 ml of ethyl 2-chloroacetoacetate and 2.75 g of calcium carbonate, and the mixture was stirred at 50° C. for 6 hours. The reaction solution was filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography, eluting with a 5:1 mixture of toluene and ethyl acetate to give 5.65 g (yield 71%) of the title compound.

후처리

  1. filtrationThe reaction solution was filtered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was purified by silica gel column chromatography
  4. washeluting with a 5:1 mixture of toluene and ethyl acetate

출처 및 근거

ORD 기록
ord-2abacfe40f3c4aa187382bbd926eb771
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05663162

연결된 노트

불러오는 중…