Ammonia → HCID 20393354, 화합물

HRID 1863079노트

반응식

HRID 1863079 반응식
[CH2:1]([N:3]([CH2:27][CH3:28])[CH2:4][CH2:5][N:6]([CH3:26])[C:7](=[O:25])[C:8]([C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=1[C:17](=O)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=O)[CH3:2].N.C([BH3-])#[N:31].[Na+]>>[ClH:16].[CH2:1]([N:3]([CH2:27][CH3:28])[CH2:4][CH2:5][N:6]([CH3:26])[C:7]([C:8]1[NH:31][C:17]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[C:11]2[C:10]=1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12]2)=[O:25])[CH3:2]

참가 물질

4

반응물 3

HCID 222AmmoniaHCID 5003444Sodium cyanoborohydrideHCID 20393335HCID 20393335, 화합물

생성물 1

HCID 20393354HCID 20393354, 화합물

실험 절차

In accordance with the procedure described in Example 3, 16.0 g. of o-benzoyl-p-chlorophenylglyoxylic acid [2-(diethylamino)ethyl]methylamide are reacted with 4.1 g. of ammonia and 1.6 g. of sodium cyanoborohydride. The ether extract containing the free base is concentrated to about 300 ml. and treated with ethereal hydrochloric acid. The precipitated hydrochloride is recrystallized from ethanol, and there is obtained 5-chloro-3-phenylisoindole-1-carboxylic acid [2-(diethylamino)ethyl]methylamide hydrochloride in the form of felt-like greenish crystals having a melting point of 208°-210° C. (decomposition).

후처리

  1. extractionThe ether extract
  2. additioncontaining the free base
  3. concentrationis concentrated to about 300 ml
  4. additionand treated with ethereal hydrochloric acid
  5. customThe precipitated hydrochloride is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-729e83bffcb14033ab91796ea797da8f
출처 데이터셋
uspto-grants-1979_09
특허 번호
US04167632

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