Phosphoric Acid → Desvenlafaxine

HRID 860914

反応式

HRID 860914 の反応式
[CH3:1][N:2]([CH2:4][CH:5]([C:14]1([OH:20])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)[C:6]1[CH:7]=[CH:8][C:9]([O:12]C)=[CH:10][CH:11]=1)[CH3:3].[Na].C1(S)C=CC=CC=1.OP(O)(O)=O>O>[CH3:1][N:2]([CH2:4][CH:5]([C:14]1([OH:20])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)[C:6]1[CH:7]=[CH:8][C:9]([OH:12])=[CH:10][CH:11]=1)[CH3:3]

参加物

5

反応物 3

HCID 1004Phosphoric AcidHCID 5656VenlafaxineHCID 66586497SODIUM THIOPHENOXIDE

生成物 1

HCID 125017Desvenlafaxine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
160 °C

実験手順

Venlafaxine (5.6 g) and benzenethiol sodium salt (6.9 g) are charged to PEG 400 (25 g). The reaction mixture is heated to 160° C. for 5 hours. Then the temperature is lowered and water is added (60 g). The pH is adjusted to 3.5 with H3PO4. The organic by-products are removed by extraction with heptanes (25 g). The pH of the aqueous layer is then adjusted to 9.5 with aqueous ammonia. The precipitate is collected by suction filtration, re-slurried in water (100 g), isolated by suction filtration and dried in vacuo.

後処理

  1. customThe organic by-products are removed by extraction with heptanes (25 g)
  2. filtrationThe precipitate is collected by suction filtration, re-slurried in water (100 g)
  3. customisolated by suction filtration
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-45fafbe0bbc64b9b947cd0b54ba8fe40
出典データセット
uspto-grants-2006_12
特許番号
US07154001B2

関連ノート

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