Methanol → HCID 19792172、化合物

HRID 653710ノート

反応式

HRID 653710 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 19792172HCID 19792172、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-a6e06ebe3c2344b990394083d2732246
出典データセット
uspto-grants-1992_07
特許番号
US05128356

反応ノート

読み込み中…