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Sodium Hydroxide → HCID 21105647、化合物

HRID 1354767
ノート
印刷プレビュー

反応式

HRID 1354767 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:14][CH2:13][CH:12]([NH:15][C:16](=[O:22])OC(C)(C)C)[CH2:11]2)=[CH:6][CH:5]=1)([O-])=O.P([O-])([O-])([O-])=O.[Na+].[Na+].[Na+].Cl[CH2:32][CH2:33][CH2:34]C(Cl)=O.[OH-].[Na+]>C(#N)C.O>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([N:10]2[CH2:14][CH2:13][C@@H:12]([N:15]3[CH2:34][CH2:33][CH2:32][C:16]3=[O:22])[CH2:11]2)=[CH:8][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 14798Sodium Hydroxide2 回HCID 24243Trisodium PhosphateHCID 783704-Chlorobutyryl chlorideHCID 21918751HCID 21918751、化合物

生成物 1

HCID 21105647HCID 21105647、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6342
Acetonitrile
溶媒

実験手順

tert-Butyl [1-(4-Nitrophenyl)pyrrolidin-3-yl]carbamate was treated by method G. The crude product (1.4 g) was dissolved in acetonitrile (20 ml) and mixed with trisodium phosphate (0.67 g) and 4-chlorobutyryl chloride (1.1 g). After 2 hours, sodium hydroxide (0.6 g) in water (10 ml) was added and the mixture was vigorously stirred. After 12 hours, the same amount of sodium hydroxide solution was again added, and the mixture was stirred for a further 24 hours. The concentrated reaction solution was partitioned between water and-ethyl acetate, and the organic phase was dried and concentrated. The residue was hydrogenated by method B. This resulted in the product with the molecular weight of 245.33 (C14H19N3O); MS (ESI): 246 (M+H+).

後処理

  1. waitAfter 12 hours
  2. stirringthe mixture was stirred for a further 24 hours
  3. customThe concentrated reaction solution
  4. customwas partitioned between water
  5. dry with material-ethyl acetate, and the organic phase was dried
  6. concentrationconcentrated
  7. customThis resulted in the product with the molecular weight of 245.33 (C14H19N3O)

出典と根拠

ORDレコード
ord-9cb6c42eb71b4ad795feefb6e77075f8
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07223788B2

反応ノート

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