Acetic Acid → HCID 178441732, 화합물

HRID 1110051

반응식

HRID 1110051 반응식
[CH2:1]([C:5]1[N:10]=[C:9]([CH3:11])[NH:8][C:7](=[O:12])[C:6]=1[CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[C:26]2[N:30](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[N:29]=[N:28][N:27]=2)=[CH:16][CH:15]=1)[CH2:2][CH2:3][CH3:4].C1C=CC2C(C3C=CC(O)=CC=3)(C3C=CC(O)=CC=3)OC(=O)C=2C=1.[OH-].[Na+].C(O)(=O)C>CO>[CH2:1]([C:5]1[N:10]=[C:9]([CH3:11])[NH:8][C:7](=[O:12])[C:6]=1[CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[C:26]2[NH:30][N:29]=[N:28][N:27]=2)=[CH:16][CH:15]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 4764PhenolphthaleinHCID 14798Sodium HydroxideHCID 1355187986-butyl-2-methyl-5-[(2'-(N-triphenylmethyl-tetrazol-5-yl)biphen-4-yl)methyl]pyrimidin-4(3H)-one

생성물 1

HCID 178441732HCID 178441732, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The title compound may be prepared by dissolving 6-butyl-2-methyl-5-[(2'-(N-triphenylmethyl-tetrazol-5-yl)biphen-4-yl)methyl]pyrimidin-4(3H)-one in methanol and adding excess concentrated HC1 and stirring for 10-30 minutes. An indicator quantity of phenolphthalein is added followed by 10% NaOH solution until pink. Excess acetic acid is added and the mixture is extracted three times with ether. The combined organic material is dried over MgSO4, stripped of solvent in vacuo, and MPLC'd to give the title compound.

후처리

  1. additionadding excess concentrated HC1
  2. extractionthe mixture is extracted three times with ether
  3. dry with materialThe combined organic material is dried over MgSO4

출처 및 근거

ORD 기록
ord-bab9d5856177492c8e4dd039e9b2d2f3
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05324729

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