Phosphoric Acid → Desvenlafaxine

HRID 860914

반응식

HRID 860914 반응식
[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]

참가 물질

5

반응물 3

HCID 1004Phosphoric AcidHCID 5656VenlafaxineHCID 66586497SODIUM THIOPHENOXIDE

생성물 1

HCID 125017Desvenlafaxine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
160 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-45fafbe0bbc64b9b947cd0b54ba8fe40
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07154001B2

연결된 노트

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