Toluene → N'-t-butyl-N-pyrenonecarbonyl-N'-(3-toluoyl)hydrazine

HRID 21673

반응식

HRID 21673 반응식
Cl.[C:2]([NH:6][NH2:7])([CH3:5])([CH3:4])[CH3:3].[C:8]1(=[O:27])[C:21]2[C:22]3=[C:23]4[C:18](=[CH:19][CH:20]=2)[CH:17]=[CH:16][CH:15]=[C:14]4[CH:13]=[CH:12][C:11]3=[CH:10][CH:9]1[C:24](Cl)=[O:25].CC[O:30][CH2:31][CH3:32].CCCCCC.[C:39]1([CH3:45])[CH:44]=C[CH:42]=[CH:41][CH:40]=1>[OH-]>[C:2]([N:6]([C:31]([C:32]1[CH:44]=[C:39]([CH3:45])[CH:40]=[CH:41][CH:42]=1)=[O:30])[NH:7][C:24]([CH:9]1[CH:10]=[C:11]2[C:22]3=[C:23]4[C:18]([CH:17]=[CH:16][CH:15]=[C:14]4[CH:13]=[CH:12]2)=[CH:19][CH:20]=[C:21]3[C:8]1=[O:27])=[O:25])([CH3:5])([CH3:4])[CH3:3]

참가 물질

7

반응물 5

HCID 1140TolueneHCID 3283Diethyl EtherHCID 8058HexaneHCID 81889tert-Butylhydrazine monohydrochlorideHCID 131717420Pyrenonecarbonyl chloride

생성물 1

HCID 131717419N'-t-butyl-N-pyrenonecarbonyl-N'-(3-toluoyl)hydrazine

시약·촉매·용매 1

HCID 961Hydroxide용매

실험 절차

To a stirred suspension of t-butyl hydrazine hydrochloride (0.02 mol) in toluene (20 ml) and aqueous hydroxide (5 ml of 50% solution) at room temperature was added pyrenonecarbonyl chloride (0.01 mol). After stirring the reaction mixture for 20 minutes, ether and hexane were added and the solid product was filtered and washed with water. The solid product (0.5 g) was stirred in toluene (10 ml) and aqueous sodium hydroxide and m-toluoyl chloride (0.8 g) was added dropwise. After stirring for 5 hours, hexane and ether were added and the solid product filtered and air dried.

후처리

  1. filtrationthe solid product was filtered
  2. washwashed with water
  3. stirringThe solid product (0.5 g) was stirred in toluene (10 ml)
  4. additionaqueous sodium hydroxide and m-toluoyl chloride (0.8 g) was added dropwise
  5. stirringAfter stirring for 5 hours
  6. additionhexane and ether were added
  7. filtrationthe solid product filtered
  8. customair dried

출처 및 근거

ORD 기록
ord-4ace12a6e29447b3bbd6b021605bd28a
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424333

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