Hydrochloric Acid → 6-{1-Hydroxy-4-[bis-chloroethyl-amino]butyl}-3,4-dihydrocarbostyril

HRID 2291184ノート

反応式

HRID 2291184 の反応式
[O:1]=[C:2]([C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][CH:22]=1)[NH:19][C:18](=[O:23])[CH2:17][CH2:16]2)[CH2:3][CH2:4][CH2:5][N:6]([CH2:10][CH2:11][Cl:12])[CH2:7][CH2:8][Cl:9].[BH4-].[Na+].Cl.[OH-].[Na+]>CO.O>[OH:1][CH:2]([C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][CH:22]=1)[NH:19][C:18](=[O:23])[CH2:17][CH2:16]2)[CH2:3][CH2:4][CH2:5][N:6]([CH2:10][CH2:11][Cl:12])[CH2:7][CH2:8][Cl:9]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 202294206-{1-Oxo-4-[di-(2-chloroethyl)-amino]butyl}-3,4-dihydrocarbostyril

生成物 1

HCID 202294566-{1-Hydroxy-4-[bis-chloroethyl-amino]butyl}-3,4-dihydrocarbostyril

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

2.5 Grams of 6-{1-oxo-4-[di-(2-chloroethyl)-amino]butyl}-3,4-dihydrocarbostyril was dissolved in 80 ml of methanol, with stirring at a room temperature condition 1.6 g of sodium borohydride was added gradually to the mixture in 15 minutes and further stirred at a room temperature for 2 hours. To the reaction mixture was added 5 ml of concentrated hydrochloric acid was added and the reaction mixture was concentrated under a reduced pressure to dryness. The residue thus obtained was dissolved in 10 ml of water, the pH of the solution was adjusted to 6-7 by adding 2N-sodium hydroxide aqueous solution and stirred to precipitate crystals. The crystals were collected by filtration washed with water and dried to obtain 1.4 g of 6-{1-hydroxy-4-[bis(2-chloroethyl)amino]-butyl}-3,4-dihydrocarbostyril in colorless powdery product.

後処理

  1. additionwas added gradually to the mixture in 15 minutes
  2. additionwas added
  3. concentrationthe reaction mixture was concentrated under a reduced pressure to dryness
  4. customThe residue thus obtained
  5. stirringstirred
  6. customto precipitate crystals
  7. filtrationThe crystals were collected by filtration
  8. washwashed with water
  9. customdried

出典と根拠

ORDレコード
ord-88745cedd2214f31a12f577a76246a5a
出典データセット
uspto-grants-1986_10
特許番号
US04619932

反応ノート

読み込み中…