Methanol → HCID 19792172, 화합물

HRID 653710노트

반응식

HRID 653710 반응식
[CH2:1]([C:5]1[N:9]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]#[N:24])=[CH:13][CH:12]=2)[C:8]2[C:25]([C:29](OC)=[O:30])=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4].CO>O1CCCC1>[CH2:1]([C:5]1[N:9]([CH2:10][C:11]2[CH:12]=[CH:13][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]#[N:24])=[CH:15][CH:16]=2)[C:8]2[C:25]([CH2:29][OH:30])=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 887MethanolHCID 18693194Methyl 2-butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]benzimidazole-7-carboxylate

생성물 1

HCID 19792172HCID 19792172, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl 2-butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]benzimidazole-7-carboxylate (10 g) and NaBH. (2.2 g) in tetrahydrofuran (100 ml) was added dropwise methanol (19 ml) during 80 minutes. The mixture was heated for 27 further hours under reflux, and the reaction mixture was concentrated to dryness. To the concentrate was added water, which was neutralized with conc. HCl. Crystals thus separated were collected by filtration. Recrystallization from methanol afforded colorless needles (8.8 g, 93%), m.p. 203°-204° C.

후처리

  1. temperatureThe mixture was heated for 27 further hours
  2. temperatureunder reflux
  3. concentrationthe reaction mixture was concentrated to dryness
  4. additionTo the concentrate was added water, which
  5. customCrystals thus separated
  6. filtrationwere collected by filtration
  7. customRecrystallization from methanol afforded colorless needles (8.8 g, 93%), m.p. 203°-204° C.

출처 및 근거

ORD 기록
ord-a6e06ebe3c2344b990394083d2732246
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05128356

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