Sodium Hydroxide → Sri 62320

HRID 1272585

反応式

HRID 1272585 の反応式
C([O:5][C:6](=[O:34])[CH2:7][C:8](=[O:33])[CH2:9][C@H:10]([OH:32])[CH:11]=[CH:12][C:13]1[N:14]([CH:29]([CH3:31])[CH3:30])[C:15]2[C:20]([C:21]=1[C:22]1[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=1)=[CH:19][CH:18]=[CH:17][CH:16]=2)(C)(C)C.[OH-].[Na+:36]>C(O)C>[F:28][C:25]1[CH:24]=[CH:23][C:22]([C:21]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[N:14]([CH:29]([CH3:31])[CH3:30])[C:13]=2/[CH:12]=[CH:11]/[C@@H:10]([OH:32])[CH2:9][C@@H:8]([OH:33])[CH2:7][C:6]([O-:34])=[O:5])=[CH:27][CH:26]=1.[Na+:36]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 69236475HCID 69236475、化合物

生成物 1

HCID 23663976Sri 62320

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To 30 g of ester E)-(S)-7-[3-(4-Fluoro-phenyl)-1-isopropyl-1H-indol-2-yl]-5-hydroxy-3-oxo-hept-6-enoic acid tert-butyl ester in 150 ml of ethanol is added under stirring 63 ml of sodium hydroxide solution while maintaining the temperature below 12° C. The solution is stirred for 1 hour, the mixture is concentrated at 25 mm Hg and 45° C., then 220 ml of water are added, destination is continued to a remaining volume of 100 ml , then 280 ml of water are added and the solution is washed with a total of 450 ml of MTBE in 3 portions. The aquous layer is concentrated at 25 mm Hg and 45° C. to a volume of about 200 ml, 150 ml water are added, and the clear aquous solution is lyophylized over 3 days. MS: 433.21

後処理

  1. temperaturewhile maintaining the temperature below 12° C
  2. concentrationthe mixture is concentrated at 25 mm Hg and 45° C.
  3. addition220 ml of water are added
  4. addition280 ml of water are added
  5. washthe solution is washed with a total of 450 ml of MTBE in 3 portions
  6. concentrationThe aquous layer is concentrated at 25 mm Hg and 45° C. to a volume of about 200 ml, 150 ml water
  7. additionare added
  8. waitthe clear aquous solution is lyophylized over 3 days

出典と根拠

ORDレコード
ord-20dc132a521343d3bdb104d7fd74e3c2
出典データセット
uspto-grants-2007_04
特許番号
US07208623B2

関連ノート

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