Triethylamine → Voriconazole

HRID 1099523ノート

反応式

HRID 1099523 の反応式
[CH3:1][C@H:2]([C@@:10]([OH:25])([C:17]1[CH:18]=[CH:19][C:20]([F:24])=[CH:21][C:22]=1[F:23])[CH2:11][N:12]1[N:16]=[CH:15][N:14]=[CH:13]1)[C:3]1[N:8]=[CH:7][N:6]=[CH:5][C:4]=1[F:9].[C@@]12(CS([O-])(=O)=O)C(C)(C)C(CC1)CC2=O.C(N(CC)CC)C>O>[CH3:1][C@H:2]([C@@:10]([OH:25])([C:17]1[CH:18]=[CH:19][C:20]([F:24])=[CH:21][C:22]=1[F:23])[CH2:11][N:12]1[N:16]=[CH:15][N:14]=[CH:13]1)[C:3]1[N:8]=[CH:7][N:6]=[CH:5][C:4]=1[F:9]

参加物

4

反応物 2

HCID 8471TriethylamineHCID 86626425Voriconazole (1R)-(-)-10-camphorsulfonate

生成物 1

HCID 71616Voriconazole収率 78.78%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
22.5 °C

実験手順

Voriconazole (1R)-(−)-10-camphorsulfonate (1 g, 1.72 mmol) was suspended in deionised water (10 ml) and treated with triethylamine (0.24 ml, 1.72 mmol) at 45-55° C. for 3 hours and 30 minutes. The suspension was cooled down to 20-25° C., stirred for 15 minutes and filtered. The cake was washed with deionised water (15 ml). The solid was dried under vacuum at 50-60° C. until constant weight (0.473 g, 78.78% yield).

後処理

  1. filtrationfiltered
  2. washThe cake was washed with deionised water (15 ml)
  3. customThe solid was dried under vacuum at 50-60° C. until constant weight (0.473 g, 78.78% yield)

出典と根拠

ORDレコード
ord-86d788604f384c36b7d8e622b39ee172
出典データセット
uspto-grants-2012_03
特許番号
US08143397B2

反応ノート

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