Ammonia → N-tert.butyl-3,5-dibromo-2-hydroxy-benzylamine hydrochloride

HRID 616410

반응식

HRID 616410 반응식
[Br:1][C:2]1[CH:9]=[C:8]([Br:10])[CH:7]=[C:4]([CH:5]=O)[C:3]=1[OH:11].[C:12]([NH2:16])([CH3:15])([CH3:14])[CH3:13].N.[ClH:18]>C(O)C.CCOCC.C(O)=O>[ClH:18].[C:12]([NH:16][CH2:5][C:4]1[CH:7]=[C:8]([Br:10])[CH:9]=[C:2]([Br:1])[C:3]=1[OH:11])([CH3:15])([CH3:14])[CH3:13]

참가 물질

8

반응물 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 6385Tert-ButylamineHCID 70243,5-Dibromosalicylaldehyde

생성물 1

HCID 20308288N-tert.butyl-3,5-dibromo-2-hydroxy-benzylamine hydrochloride

시약·촉매·용매 3

HCID 284Formic Acid용매HCID 702Ethanol용매HCID 3283Diethyl Ether용매

실험 절차

7 gm of 3,5-dibromo-salicylaldehyde, 17.5 gm of tert. butylamine and 7.7 gm of formic acid were heated for 6 hours at 70°-80° C. Subsequently, the reaction mixture was admixed with aqueous 2 N ammonia, vigorously shaken, and the precipitate formed thereby was sucked off. The residue was dissolved in ethanol, acidified with ethanolic hydrochloric acid and admixed with ether in order to crystallize the product out. N-tert.butyl-3,5-dibromo-2-hydroxy-benzylamine hydrochloride, m.p. 216°-220° C (decomp.), was obtained after recrystallization from absolute ethanol/ether.

후처리

  1. customthe precipitate formed
  2. customto crystallize the product out

출처 및 근거

ORD 기록
ord-3136111fc16f4cebb7a7f3363b4d7f1b
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04073942

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