Glycine ethyl ester → HCID 21285524, 화합물

HRID 2231653노트

반응식

HRID 2231653 반응식
[NH2:1][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].[NH2:8][C:9]1[C:16]([CH3:17])=[CH:15][C:14]([I:18])=[CH:13][C:10]=1[CH:11]=O>C(Cl)(Cl)Cl>[NH2:8][C:9]1[C:16]([CH3:17])=[CH:15][C:14]([I:18])=[CH:13][C:10]=1[CH2:11][NH:1][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4]

참가 물질

4

반응물 2

HCID 12176Glycine ethyl esterHCID 212855162-Amino-5-iodo-3-methylbenzaldehyde

생성물 1

HCID 21285524HCID 21285524, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of freshly prepared ethyl glycinate (2.58 g), 2-amino-5-iodo-3-methylbenzaldehyde (4.03 g) and 3Å molecular sieves (2 g "Fluka A.G." [Trade Mark] article No. 69828) was heated with stirring under reflux in chloroform (50 cm3) for 4 hours. The cooled solution was filtered, evaporated in vacuo, and the residue taken into ethanol (30 cm3) and treated with sodium cyanoborohydride (1.43 g). After stirring for 72 hours ethanol was removed in vacuo and the residue was partitioned between chloroform (50 cm3) and aqueous ammonia (50 cm3, S.G. 0.88). The aqueous phase was further extracted with chloroform (2×100 cm3) and the combined organic extracts were dried (MgSO4) and evaporated to give the title compound as a crude oil, (2.5 g).

후처리

  1. temperature69828) was heated
  2. filtrationThe cooled solution was filtered
  3. customevaporated in vacuo
  4. additiontreated with sodium cyanoborohydride (1.43 g)
  5. stirringAfter stirring for 72 hours ethanol
  6. customwas removed in vacuo
  7. customthe residue was partitioned between chloroform (50 cm3) and aqueous ammonia (50 cm3, S.G. 0.88)
  8. extractionThe aqueous phase was further extracted with chloroform (2×100 cm3)
  9. dry with materialthe combined organic extracts were dried (MgSO4)
  10. customevaporated

출처 및 근거

ORD 기록
ord-7730e126de544f6dbe4de3a940aea8b3
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04783467

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