Glycine ethyl ester → HCID 21285524、化合物

HRID 2231653ノート

反応式

HRID 2231653 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 21285524HCID 21285524、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-7730e126de544f6dbe4de3a940aea8b3
出典データセット
uspto-grants-1988_11
特許番号
US04783467

反応ノート

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