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Hydrazine hydrate (1:1) → 12-Amino-1-dodecanol

HRID 1003308
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HRID 1003308 반응식
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][N:14]1C(=O)C2=CC=CC=C2C1=O.O.NN>CO>[NH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][OH:1]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 18796407N-(12-hydroxydodecyl)phthalimide

생성물 1

HCID 518202012-Amino-1-dodecanol수율 74.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In 600 ml of methanol was dissolved while warming 48.0 g of N-(12-hydroxydodecyl)phthalimide, 50 ml of hydrazine monohydrate was added at room temperature with stirring and the mixture was stirred overnight. The crystal thus separated out was filtered off and the solvent was distilled off. The residue was extracted with hot chloroform and insolubles were filtered off. The filtrate was distilled, the residue was extracted with hot chloroform (100 ml×3) and then the solvent was distilled off. The residue was dissolved in methanol and recrystallization from methanol-ethyl acetate gave 21.6 g of the title compound as a crystal.

후처리

  1. additionwas added at room temperature
  2. stirringthe mixture was stirred overnight
  3. customThe crystal thus separated out
  4. filtrationwas filtered off
  5. distillationthe solvent was distilled off
  6. extractionThe residue was extracted with hot chloroform and insolubles
  7. filtrationwere filtered off
  8. distillationThe filtrate was distilled
  9. extractionthe residue was extracted with hot chloroform (100 ml×3)
  10. distillationthe solvent was distilled off
  11. dissolutionThe residue was dissolved in methanol
  12. customrecrystallization from methanol-ethyl acetate

출처 및 근거

ORD 기록
ord-c7baf5ca20614e9b99493d1848dede8b
출처 데이터셋
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06046201

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