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Hydrochloric Acid → Ethyl 3-(4-(2-tetrazolyl)-phenylhydrazino)-4-oxopentanoate

HRID 399419
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HRID 399419 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[N:12]=[N:11][CH:10]=[N:9]2)=[CH:4][CH:3]=1.Cl.[N:14]([O-])=O.[Na+].[C:18]([CH:21](C(=O)C)[CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])(=[O:20])[CH3:19]>C(O)C.N1C=CC=CC=1.O>[N:9]1[N:8]([C:5]2[CH:4]=[CH:3][C:2]([NH:1][NH:14][CH:21]([C:18](=[O:20])[CH3:19])[CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])=[CH:7][CH:6]=2)[N:12]=[N:11][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 87820Ethyl 3-acetyl-4-oxopentanoateHCID 5716394-(2H-1,2,3,4-tetrazol-2-yl)anilineHCID 23668193Sodium Nitrite

생성물 1

HCID 53974079Ethyl 3-(4-(2-tetrazolyl)-phenylhydrazino)-4-oxopentanoate

시약·촉매·용매 3

HCID 702Ethanol용매2회
HCID 962Water용매3회
HCID 1049Pyridine용매

실험 절차

A solution of 1.06 gm. (6.58 mmoles) of 2-(4-aminophenyl)tetrazole in 20 ml. of ethanol and 1.18 ml. of concentrated hydrochloric acid and 10 ml. of water was cooled in an ice bath and treated dropwise with a solution of 500 mg. of sodium nitrite in 10 ml. of water. After the addition of an additional 10 ml. of water, the mixture was stirred for 25 minutes at room temperature. The mixture was then added to a solution of 1.35 gm. (7.2 mmoles) of ethyl 3-acetyl-4-oxopentanoate and 2.66 ml. of pyridine in 15 ml. of ethanol. A solid began to separate. After 1 hour, 10 ml. of 1 M hydrochloric acid was added to adjust the pH to 2-3. An additional 50 ml. of water was added and the solid was collected and washed thoroughly with water and dried. 1.74 g. was obtained.

후처리

  1. additiontreated dropwise with a solution of 500 mg
  2. additionAfter the addition of an additional 10 ml
  3. additionThe mixture was then added to a solution of 1.35 gm
  4. customto separate
  5. additionof 1 M hydrochloric acid was added
  6. additionof water was added
  7. customthe solid was collected
  8. washwashed thoroughly with water
  9. customdried
  10. customwas obtained

출처 및 근거

ORD 기록
ord-6b64e15b64cd411dad25059c24699d8a
출처 데이터셋
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05821243

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