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Lithium Hydroxide → HCID 16103460, 화합물

HRID 83965
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HRID 83965 반응식
C([O:3][C:4]([C:6]1[S:13][C:12]2[C:11]3[S:14][C:15]4[C:19]([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[C:18]([C:30]([O:32]CC)=[O:31])[S:17][C:16]=4[C:10]=3[S:9][C:8]=2[C:7]=1[CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44])=[O:5])C.[Li+].[OH-].C1COCC1>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.CO>[CH2:20]([C:19]1[C:15]2[S:14][C:11]3[C:12]4[S:13][C:6]([C:4]([OH:5])=[O:3])=[C:7]([CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44])[C:8]=4[S:9][C:10]=3[C:16]=2[S:17][C:18]=1[C:30]([OH:32])=[O:31])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 16103489Diethyl 3,7-didecylthieno[3,2-b]thieno[2',3':4,5]thieno[2,3-d]thiophene 2,6-dicarboxylate

생성물 1

HCID 16103460HCID 16103460, 화합물수율 97.4%

시약·촉매·용매 2

HCID 67553Tetrabutylammonium Iodide촉매
HCID 887
Methanol
용매

실험 절차

Compound 74 (14.0 g, 0.021 mol) is mixed with LiOH (1.24 g, in 15 mL water), THF (100 mL), MeOH (20 mL) and a catalytic amount of tetrabutylammonium iodide. This mixture is heated at reflux overnight and most of the solvent is evaporated. The residue is acidified with concentrated HCl (30 mL). The resultant solid is collected by filtration, washed thoroughly with water and vacuum dried to yield compound 75 (12.5 g, 97.4% yield). M.P.: 315.6-318.5° C.

후처리

  1. temperatureThis mixture is heated
  2. temperatureat reflux overnight and most of the solvent
  3. customis evaporated
  4. filtrationThe resultant solid is collected by filtration
  5. washwashed thoroughly with water and vacuum
  6. customdried

출처 및 근거

ORD 기록
ord-f0058e8e041c49768232c4fa11e82164
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846855B2

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