Isobutyl chloroformate → HCID 178512905、化合物

HRID 1679645ノート

反応式

HRID 1679645 の反応式
[NH2:1][C@H:2]([C:10]([OH:12])=O)[CH2:3][CH2:4][CH2:5][NH:6][C:7](=[NH:9])[NH2:8].C(OC(N([N+]([O-])=O)[C@H](C(O)=O)CCCNC(=N)N)=O)(C)(C)C.C(Cl)(=O)OCC(C)C.[NH2:43][CH2:44][C:45]([NH2:47])=[O:46]>CN(C)C=O.O1CCCC1.C(N(CC)CC)C>[NH2:1][C@H:2]([C:10]([NH:43][CH2:44][C:45]([NH2:47])=[O:46])=[O:12])[CH2:3][CH2:4][CH2:5][NH:6][C:7](=[NH:9])[NH2:8]

参加物

8

反応物 4

HCID 62365Isobutyl chloroformateHCID 69020GlycinamideHCID 178418600HCID 178418600、化合物HCID 178454196HCID 178454196、化合物

生成物 1

HCID 178512905HCID 178512905、化合物

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒2 回HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒

実験手順

Protected arginine, i.e., tert-butyloxycarbonylnitro-arginine is dissolved in a suitable solvent such as dimethylformamide and tetrahydrofuran. The dissolved protected amino acid is then cooled to a temperature slightly below the freezing point (0° C), whereupon isobutyl chlorocarbonate and triethylamine is added with stirring. After a short period, glycinamide dissolved in dimethylformamide is added. The mixture is then permitted to warm to room temperature and stirred for a period of several hours and then filtered. The filtrate is recovered and evaporated to dryness and then extracted with dimethylformamide. The dimethylformamide solution is precipitated with ethylacetate to yield the dipeptide, i.e., protected arginyl-glycinamide.

後処理

  1. additionis added
  2. waitAfter a short period
  3. additionis added
  4. stirringstirred for a period of several hours
  5. filtrationfiltered
  6. customThe filtrate is recovered
  7. customevaporated to dryness
  8. extractionextracted with dimethylformamide
  9. customThe dimethylformamide solution is precipitated with ethylacetate

出典と根拠

ORDレコード
ord-55a5380ecac242509ecaf254a4a52585
出典データセット
uspto-grants-1978_03
特許番号
US04081533

反応ノート

読み込み中…