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Hydrochloric Acid → Ethyl 2-amino-2-(10,11-dihydro-5H-dibenzo[a,d][7]annulen-5-yl)acetate hydrochloride

HRID 258196
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반응식

HRID 258196 반응식
[N+:1]([CH:4]([CH:10]1[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[CH:14]=[CH:13][C:12]2[CH:21]=[CH:22][CH:23]=[CH:24][C:11]1=2)[C:5]([O:7][CH2:8][CH3:9])=[O:6])([O-])=O.O.[ClH:26]>C(O)C.[Pd]>[ClH:26].[NH2:1][CH:4]([CH:10]1[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[CH2:14][CH2:13][C:12]2[CH:21]=[CH:22][CH:23]=[CH:24][C:11]1=2)[C:5]([O:7][CH2:8][CH3:9])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 15290760Ethyl alpha-nitro-5H-dibenzo[a,d]cycloheptene-5-acetate

생성물 1

HCID 19385933Ethyl 2-amino-2-(10,11-dihydro-5H-dibenzo[a,d][7]annulen-5-yl)acetate hydrochloride

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol
용매

실험 절차

Ethyl α-nitro-5H-dibenzo[a,d]cycloheptene-5-acetate (13 g, 40 mmol) (Example 4, Step A) is dissolved in 150 mL of ethanol, 40 mL of water, and 3.5 mL of concentrated hydrochloric acid and hydrogenated with 2.0 g of 20% palladium on carbon (52 psi, 30 hours). The filtered solution is stripped and a white solid washed with diethyl ether, dried at 50° C./2 mm Hg. The crude product is used as is in the next step.

후처리

  1. washa white solid washed with diethyl ether
  2. customdried at 50° C./2 mm Hg

출처 및 근거

ORD 기록
ord-60d4a1eac74e4c15ab2aa7f26df34e18
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05264577

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