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Ammonium Chloride → HCID 44545376、化合物

HRID 2387336
ノート
印刷プレビュー

反応式

HRID 2387336 の反応式
C(OC(=O)[NH:7][C:8]1[CH:9]=[N:10][C:11]([S:38]([CH3:41])(=[O:40])=[O:39])=[CH:12][C:13]=1[C:14]#[C:15][CH2:16][C@@:17]([OH:37])([C:33]([F:36])([F:35])[F:34])[CH2:18][C:19]([C:22]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:23]=1[S:29]([CH3:32])(=[O:31])=[O:30])([CH3:21])[CH3:20])(C)(C)C.C1CCN2C(=NCCC2)CC1.[Cl-].[NH4+]>CO>[Cl:28][C:25]1[CH:26]=[CH:27][C:22]([C:19]([CH3:21])([CH3:20])[CH2:18][C@:17]([CH2:16][C:15]2[NH:7][C:8]3=[CH:9][N:10]=[C:11]([S:38]([CH3:41])(=[O:40])=[O:39])[CH:12]=[C:13]3[CH:14]=2)([OH:37])[C:33]([F:36])([F:35])[F:34])=[C:23]([S:29]([CH3:32])(=[O:30])=[O:31])[CH:24]=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

5

反応物 3

HCID 25517Ammonium ChlorideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 58026125HCID 58026125、化合物

生成物 1

HCID 44545376HCID 44545376、化合物収率 99.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

To a solution of the {4-[(S)-6-(4-chloro-2-methanesulfonylphenyl)-4-hydroxy-6-methyl-4-trifluoromethylhept-1-ynyl]-6-methanesulfonylpyridin-3-yl}carbamic acid tert-butyl ester (18.3 g, 28.0 mmol) in 200 mL of methanol was added DBU (12.5 mL, 84.0 mmol). The reaction was heated to 70° C. for 1.5 hours. The reaction was added to a solution of saturated aqueous ammonium chloride solution resulting in the precipitation of a white solid that was collected by vacuum filtration. The solid was washed with water and, after drying under vacuum for 30 minutes, was suspended in 50 mL of cold diethyl ether then vacuum filtered again and washed with 50 mL of cold diethyl ether. The colorless solid was dried on the filter paper under suction to provide (R)-4-(4-chloro-2-methanesulfonylphenyl)-1,1,1-trifluoro-2-(5-methanesulfonyl-1H-pyrrolo[2,3-c]pyridin-2-ylmethyl)-4-methylpentan-2-ol (15.4 g, 99%).

後処理

  1. customresulting in the precipitation of a white solid
  2. filtrationthat was collected by vacuum filtration
  3. washThe solid was washed with water
  4. customafter drying under vacuum for 30 minutes
  5. filtrationvacuum filtered again
  6. washwashed with 50 mL of cold diethyl ether
  7. customThe colorless solid was dried on the filter paper under suction

出典と根拠

ORDレコード
ord-1118f5ee75b14fb28bd53856accc912b
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268859B2

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