Sodium Chloride → Enalapril

HRID 2242530

反応式

HRID 2242530 の反応式
[CH2:1]([O:3][C:4]([CH:6]([NH:15][C@H:16]([C:18]([OH:20])=O)[CH3:17])[CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:5])[CH3:2].[NH:21]1[CH2:28][CH2:27][CH2:26][C@H:22]1[C:23]([OH:25])=[O:24].F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.[Na+].[Cl-]>C(#N)C.CN(C=O)C.C(N(CC)CC)C>[CH3:2][CH2:1][O:3][C:4]([C@@H:6]([NH:15][C@H:16]([C:18]([N:21]1[C@H:22]([C:23]([OH:25])=[O:24])[CH2:26][CH2:27][CH2:28]1)=[O:20])[CH3:17])[CH2:7][CH2:8][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)=[O:5]

参加物

8

反応物 4

HCID 5234Sodium ChlorideHCID 145742L-ProlineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 13044262N-(1-ethoxycarbonyl-3-phenylpropyl)-L-alanine

生成物 1

HCID 5388962Enalapril

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒HCID 6342Acetonitrile溶媒HCID 8471Triethylamine溶媒

実験手順

2.9 ml triethylamine was added to the mixture of 2.79 g of 1-((S)—N-(1-(ethoxycarbonyl)-3-phenylpropyl)-L-alanine and 1.15 g of L-proline in 100 ml of acetonitrile and 5 ml DMF and during stirring 3.8 g O-(benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate was added. The reaction mixture was stirred for further 30 minutes at room temperature. 300 ml of saturated NaCl solution was added and the mixture was extracted twice with 100 ml of ethyl acetate. Combined extracts were washed with 70 ml of water/1 ml of conc. HCl mixture and then with 130 ml of water, dried with Na2SO4 and evaporated at 40° C. in vacuum. 3.55 g of enalapril was obtained.

後処理

  1. additionwas added
  2. extractionthe mixture was extracted twice with 100 ml of ethyl acetate
  3. washCombined extracts were washed with 70 ml of water/1 ml of conc. HCl mixture
  4. dry with materialwith 130 ml of water, dried with Na2SO4
  5. customevaporated at 40° C. in vacuum

出典と根拠

ORDレコード
ord-59f5c79f793146ffb64f39a00dd9ca49
出典データセット
uspto-grants-2010_03
特許番号
US07671215B2

関連ノート

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