Sodium borohydride → HCID 70434749, 화합물

HRID 1380329노트

반응식

HRID 1380329 반응식
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]

참가 물질

5

반응물 3

HCID 4311764Sodium borohydride2회HCID 20214926HCID 20214926, 화합물HCID 20214946HCID 20214946, 화합물

생성물 1

HCID 70434749HCID 70434749, 화합물수율 50.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 9.3 gm of 2,5-dichloro-4-hydroxyphenyl-glyoxal 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×1H2O, m.p. 180°-183° C., of the formula ##STR29## were obtained. The yield was 50.4% of theory.

후처리

  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

출처 및 근거

ORD 기록
ord-e6b474f54bb04834a8bd2b8216c7938e
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04581367

반응 노트

불러오는 중…