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Sodium Hydroxide → HCID 68541409, 화합물

HRID 1432123
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HRID 1432123 반응식
C[O:2][C:3](=[O:21])[C:4]1[CH:17]=[C:16]([O:18][CH2:19][CH3:20])[CH:15]=[C:6]([C:7]([N:9]([CH2:12][CH:13]=[CH2:14])[CH2:10][CH3:11])=[O:8])[CH:5]=1.[OH-].[Na+]>CO>[CH2:12]([N:9]([CH2:10][CH3:11])[C:7](=[O:8])[C:6]1[CH:5]=[C:4]([CH:17]=[C:16]([O:18][CH2:19][CH3:20])[CH:15]=1)[C:3]([OH:21])=[O:2])[CH:13]=[CH2:14]
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반응물 2

HCID 14798Sodium HydroxideHCID 68542335HCID 68542335, 화합물

생성물 1

HCID 68541409HCID 68541409, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 1.0 g (4.45 mmol) 5-ethoxy-isophthalic acid mono methyl ester, 10 ml toluene and 0.5 ml SOCl2 is treated with one drop DMF and heated to 80° C. till the evolution of gas ceases. After cooling down the mixture is evaporated, dissolved in 5 ml DCM and added to an at 0° C. stirred mixture of 10 ml 10% aqueous Na2CO3, 0.81 g (6.7 mmol) allyl ethyl amine hydrochloride (see IVb) and 5 ml DCM. After 1 h the layers are separated and the organic layer is washed with 1N HCl, brine, dried with sodium sulfate and evaporated to yield the N-allyl-5-ethoxy-N-ethyl-isophthalamic acid methyl ester. This ester is dissolved in 20 ml MeOH, treated with 15 ml 1N NaOH and stirred for 18 h. The methanol is evaporated, the residue acidified with 1N HCl and extracted with TBME. The organic layer is dried with sodium sulfate and evaporated to yield the title compound.

후처리

  1. customThe methanol is evaporated
  2. extractionextracted with TBME
  3. dry with materialThe organic layer is dried with sodium sulfate
  4. customevaporated

출처 및 근거

ORD 기록
ord-64fbd85755044a2a8f8f1ee7a0e71b5b
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612055B2

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