ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Acetone → HCID 68877555、化合物

HRID 1787840
ノート
印刷プレビュー

反応式

HRID 1787840 の反応式
[CH2:1]([O:8][C:9]1[CH:18]=[CH:17][C:16]([C:19](=[O:25])[CH:20](OCC)O)=[CH:15][C:10]=1[C:11]([O:13][CH3:14])=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:26][O:27][C:28]1[CH:33]=[CH:32][C:31]([C:34]2[N:38]=[C:37]([CH3:39])[N:36]([CH2:40][CH2:41][C:42]([NH2:45])([CH3:44])[CH3:43])[N:35]=2)=[CH:30][CH:29]=1.[BH4-].[Na+].CC(C)=O>C(O)C.C(O)(=O)C>[CH2:1]([O:8][C:9]1[CH:18]=[CH:17][C:16]([CH:19]([OH:25])[CH2:20][NH:45][C:42]([CH3:44])([CH3:43])[CH2:41][CH2:40][N:36]2[C:37]([CH3:39])=[N:38][C:34]([C:31]3[CH:30]=[CH:29][C:28]([O:27][CH3:26])=[CH:33][CH:32]=3)=[N:35]2)=[CH:15][C:10]=1[C:11]([O:13][CH3:14])=[O:12])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物反応条件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 180AcetoneHCID 4311764Sodium borohydrideHCID 59754203HCID 59754203、化合物HCID 68858509Methyl benzyloxy-5-(2-ethoxy-2-hydroxy-acetyl)-benzoate

生成物 1

HCID 68877555HCID 68877555、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒
HCID 702
Ethanol
溶媒

反応条件

温度
10 °C

実験手順

8.5 g of methyl 2-benzyloxy-5-(2-ethoxy-2-hydroxy-acetyl)-benzoate and 4.9 g of 3-[3-(4-methoxy-phenyl)-5-methyl-[1,2,4]triazol-1-yl]-1,1-dimethyl-propylamine in 100 mL ethanol are stirred for three hours at 60° C., cooled to 10° C., combined batchwise with 0.8 g of sodium borohydride and stirred for a further three hours at ambient temperature. Then 10 mL acetone are added and the mixture is stirred for one hour. It is then poured onto ice and acidified with glacial acetic acid. The ethanol is distilled off, the aqueous phase remaining is made alkaline with sodium hydroxide and extracted with ethyl acetate. The organic phases are dried with sodium sulphate and evaporated down. The residue is combined with 80 mL ethanol, acidified with 3.2 g of oxalic acid, dissolved in ethanol, and seeded. The product that crystallises out is suction filtered and washed. Yield: 8 g (69%, oxalate); m.p.=210-213° C.

後処理

  1. stirringthe mixture is stirred for one hour
  2. additionIt is then poured onto ice
  3. distillationThe ethanol is distilled off
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic phases are dried with sodium sulphate
  6. customevaporated down
  7. dissolutiondissolved in ethanol
  8. customThe product that crystallises out is suction
  9. filtrationfiltered
  10. washwashed

出典と根拠

ORDレコード
ord-9f34e6e3d751450c9ab46d4ded2de53c
出典データセット
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07511067B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート