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Water → HCID 18536711、化合物

HRID 412071
ノート
印刷プレビュー

反応式

HRID 412071 の反応式
C([O:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([NH:12][C:13]([O:15][CH2:16][C:17]2[N:18]=[CH:19][N:20]([C:22]3[CH:23]=[C:24]4[C:29](=[CH:30][C:31]=3[C:32]([F:35])([F:34])[F:33])[NH:28][C:27](=[O:36])[C:26]([C:37]([O:39]CC)=[O:38])=[CH:25]4)[CH:21]=2)=[O:14])=[CH:8][CH:7]=1)=[O:5])C.[OH-].[Li+].O>C(O)C>[C:4]([C:6]1[CH:11]=[CH:10][C:9]([NH:12][C:13]([O:15][CH2:16][C:17]2[N:18]=[CH:19][N:20]([C:22]3[CH:23]=[C:24]4[C:29](=[CH:30][C:31]=3[C:32]([F:35])([F:33])[F:34])[NH:28][C:27](=[O:36])[C:26]([C:37]([OH:39])=[O:38])=[CH:25]4)[CH:21]=2)=[O:14])=[CH:8][CH:7]=1)([OH:5])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962Water2 回HCID 3939Lithium Hydroxide2 回HCID 9808166HCID 9808166、化合物

生成物 1

HCID 18536711HCID 18536711、化合物収率 74.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of the compound of Example 18 (1.13 g, 1.97 mmol) in ethanol (30 ml) was added 1 mol/L aqueous solution of lithium hydroxide (9.26 ml, 9.26 mmol) and successively water (15 ml), and, after stirring for 4 hours at room temperature, the mixture was allowed to stand statically overnight. After stirring for 16 hours at 30° C., ice water was added to the reaction mixture and the insolubles were filtered off. Then, the pH value was brought to 4 with 3 mol/L hydrochloric acid and solvent was distilled off. Water was added to the residue obtained, the precipitated crystals were collected by filtration, washed with water, and then dried under reduced pressure. After the powder obtained was suspended into water (40 ml), 1 mol/L aqueous solution of lithium hydroxide (9.26 ml, 9.26 mmol) was added and the mixture was stirred for 30 minutes at 50° C. Ice water was added to the reaction mixture, the insolubles were filtered off, then the pH value was brought to 4 with 3 mol/L hydrochloric acid, and solvent was distilled off. Water was added to the residue obtained, the precipitated crystals were collected by filtration, washed with water, and then dried under reduced pressure, thereby obtaining 757 mg of title compound as pale yellow powder.

後処理

  1. waitto stand statically overnight
  2. stirringAfter stirring for 16 hours at 30° C.
  3. filtrationthe insolubles were filtered off
  4. distillationwas distilled off
  5. additionWater was added to the residue
  6. customobtained
  7. filtrationthe precipitated crystals were collected by filtration
  8. washwashed with water
  9. customdried under reduced pressure
  10. customAfter the powder obtained
  11. additionwas added
  12. stirringthe mixture was stirred for 30 minutes at 50° C
  13. filtrationthe insolubles were filtered off
  14. distillationwas distilled off
  15. additionWater was added to the residue
  16. customobtained
  17. filtrationthe precipitated crystals were collected by filtration
  18. washwashed with water
  19. customdried under reduced pressure

出典と根拠

ORDレコード
ord-9b7235fdbf8044478af862a9130d1fcb
出典データセット
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06562839B1

反応ノート

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