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Sodium dicyanamide → HCID 178445599, 화합물

HRID 1248454
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HRID 1248454 반응식
Cl.[F:2][C:3]([F:10])([F:9])[CH2:4][C:5]([NH2:8])([CH3:7])[CH3:6].[N-:11]([C:14]#[N:15])[C:12]#[N:13].[Na+]>C(O)CCC>[C:12]([NH:11][C:14]([NH:8][C:5]([CH3:7])([CH3:6])[CH2:4][C:3]([F:10])([F:9])[F:2])=[NH:15])#[N:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4350929Sodium dicyanamideHCID 202781154,4,4-Trifluoro-2-methylbutan-2-amine HCl

생성물 1

HCID 178445599HCID 178445599, 화합물수율 82.3%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

A mixture of 3,3,3-trifluoro-1,1-dimethylpropylamine hydrochloride (2.67 g, 15 mol), sodium dicyanamide (1.34 g, 15 mmol), and n-butanol (7.5 ml) was sealed in vacuo in a Pyrex ampoule and was heated at 105° for 119 h to give, after solvent removal, a residue (2.87 g) which was crushed and stirred with water (7 ml), then filtered and washed with water, then dried to give a solid (2.57 g) with m.p. 153° (shrinks 145°). The solid was dissolved in methanol (25 ml) then filtered to remove what is presumed to be polymeric dicyanamide (0.06 g). Removal of solvent and drying gave the guanidine (2.35 g) m.p. 153°-4°.

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후처리

  1. customwas sealed in vacuo in a Pyrex ampoule
  2. temperaturewas heated at 105° for 119 h
  3. customto give
  4. customafter solvent removal
  5. customa residue (2.87 g) which was crushed
  6. filtrationfiltered
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-29954a125b1a4fafb38085c458a2a304
출처 데이터셋
uspto-grants-1985_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04524152

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