Methanol → 3-(2-(4-((4-Fluorophenyl)hydroxymethyl)-1-piperidinyl)ethyl)-2,4(1H,3H)-quinazolinedione

HRID 1248251

반응식

HRID 1248251 반응식
[F:1][C:2]1[CH:29]=[CH:28][C:5]([C:6]([CH:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][N:16]3[C:25](=[O:26])[C:24]4[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=4)[NH:18][C:17]3=[O:27])[CH2:10][CH2:9]2)=[O:7])=[CH:4][CH:3]=1.CO.[BH4-].[Na+]>O>[F:1][C:2]1[CH:29]=[CH:28][C:5]([CH:6]([OH:7])[CH:8]2[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][N:16]3[C:25](=[O:26])[C:24]4[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=4)[NH:18][C:17]3=[O:27])[CH2:12][CH2:13]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 3822KetanserinHCID 4311764Sodium borohydride

생성물 1

HCID 1563943-(2-(4-((4-Fluorophenyl)hydroxymethyl)-1-piperidinyl)ethyl)-2,4(1H,3H)-quinazolinedione

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred mixture of 2.6 parts of 3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-2,4(1H,3H)-quinazolinedione and 120 parts of methanol are added portionwise 2 parts of sodium borohydride. Upon completion, stirring is continued overnight at room temperature. Water is added and the whole is evaporated. The residue is stirred in water. The solid product is filtered off and crystallized from 2-propanone, yielding 1.2 parts of 3-[2-[4-[(4-fluorophenyl)hydroxymethyl]-1-piperidinyl]ethyl]-2,4(1H,3H)-quinazolinedione; mp. 212.8° C.

후처리

  1. customthe whole is evaporated
  2. stirringThe residue is stirred in water
  3. filtrationThe solid product is filtered off
  4. customcrystallized from 2-propanone

출처 및 근거

ORD 기록
ord-f947b5b120344dbda0d61256c471343e
출처 데이터셋
uspto-grants-1985_06
특허 번호
US04522945

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