Sodium borohydride → HCID 70434749、化合物

HRID 355200ノート

反応式

HRID 355200 の反応式
O.[Cl:2][C:3]1[CH:8]=[C:7]([OH:9])[C:6]([Cl:10])=[CH:5][C:4]=1[C:11]([CH:13]=O)=[O:12].[NH2:15][C:16]([CH3:29])([CH3:28])[CH2:17][CH2:18][N:19]1[C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2[N:21]=[CH:20]1.[BH4-].[Na+]>CO>[ClH:2].[ClH:2].[Cl:2][C:3]1[CH:8]=[C:7]([OH:9])[C:6]([Cl:10])=[CH:5][C:4]=1[CH:11]([OH:12])[CH2:13][NH:15][C:16]([CH3:29])([CH2:17][CH2:18][N:19]1[C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2[N:21]=[CH:20]1)[CH3:28]

参加物

5

反応物 3

HCID 4311764Sodium borohydride2 回HCID 20214926HCID 20214926、化合物HCID 20214946HCID 20214946、化合物

生成物 1

HCID 70434749HCID 70434749、化合物収率 50.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 9.3 gm of 2,5-dichloro-4-hydroxyphenylglyoxal hydrate, 7.25 gm of 1-(3-amino-3-methylbutyl)-benzimidazole and 100 ml of alcohol was stirred for 3 hours at 40°-45° C. The resulting solution was subsequently cooled, admixed in portions with 8 gm of sodium borohydride, and the mixture was stirred for 3 hours at room temperature. After the addition of 100 ml of methanol for decomposition of the sodium borohydride, the mixture was allowed to stand for 10 hours, the solvent was distilled off under reduced pressure, the residue was dissolved in 200 ml of water, and the solution was acidified with concentrated hydrochloric acid. 9.5 gm of 1-(2,5-dichloro-4-hydroxyphenyl)-2-[4-(1-benzimidazolyl)-2-methyl-2-butylamino]-ethanol dihydrochloride×1 H2O, m.p. 180°-183° C., of the formula ##STR33## were obtained. The yield was 50.4% of theory.

後処理

  1. temperatureThe resulting solution was subsequently cooled
  2. stirringthe mixture was stirred for 3 hours at room temperature
  3. waitto stand for 10 hours
  4. distillationthe solvent was distilled off under reduced pressure
  5. dissolutionthe residue was dissolved in 200 ml of water
  6. customwere obtained

出典と根拠

ORDレコード
ord-2edd5ff5e4e34511bc7a7bf869ab5ac1
出典データセット
uspto-grants-1983_03
特許番号
US04378361

反応ノート

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